CN104818410B - Dental is cut processing blank material and metal powder for powder metallurgy - Google Patents
Dental is cut processing blank material and metal powder for powder metallurgy Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61C13/00—Dental prostheses; Making same
- A61C13/0003—Making bridge-work, inlays, implants or the like
- A61C13/0022—Blanks or green, unfinished dental restoration parts
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
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- A61C13/0004—Computer-assisted sizing or machining of dental prostheses
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
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- A61C13/0003—Making bridge-work, inlays, implants or the like
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- A61C13/00—Dental prostheses; Making same
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- A61C13/083—Porcelain or ceramic teeth
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- A—HUMAN NECESSITIES
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- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/84—Preparations for artificial teeth, for filling teeth or for capping teeth comprising metals or alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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Abstract
Description
技术领域technical field
本发明涉及牙科用的被切削加工用坯材、粉末冶金用金属粉末、牙科用的烤瓷用金属框架及牙科用修补物。The present invention relates to a blank material for cutting in dentistry, a metal powder for powder metallurgy, a metal frame for ceramics in dentistry and a dental prosthesis.
背景技术Background technique
在牙科治疗中,修补牙冠缺损部、牙体缺损部时,经常使用冠、桥或义齿。其中,从审美观、功能性的角度出发,可使用在金属框架的表面烤上被称为陶材的陶瓷材料而成的牙科用修补物。In dental treatment, crowns, bridges or dentures are often used to repair crown defects or tooth defects. Among them, from the viewpoints of aesthetics and functionality, dental prostheses in which a ceramic material called pottery is baked on the surface of a metal frame can be used.
在专利文献1中公开了一种对Au、Pd、Cu、Ir、Ag等金属元素加上Sn、Ga、In等金属元素的、贵金属类的金属框架用合金。由于这种合金可以通过铸造法成形为所需的形状,因此,通过在由这种合金构成的金属框架的表面烤上齿冠修复用陶材,从而可以得到审美性良好的牙科用修补物。Patent Document 1 discloses a precious metal alloy for metal frames in which metal elements such as Sn, Ga, and In are added to metal elements such as Au, Pd, Cu, Ir, and Ag. Since this alloy can be formed into a desired shape by casting, a dental prosthesis with good aesthetics can be obtained by baking a ceramic material for tooth crown restoration on the surface of a metal frame made of this alloy.
另一方面,最近,测定患部的立体形状,并根据所得的形状数据形成金属框架的方法正在普及。这种结构被称为牙科CAD/CAM系统。CAD(computer aided design,计算机辅助设计)是通过3D扫描等取得患部的立体形状并将其数值化的系统。而且,CAM(computeraided design,计算机辅助制造)是根据由CAD生成的数值数据,对被加工物实施切削加工,切出形状适合于患部的金属框架的系统。由于将这些系统组合后的牙科CAD/CAM系统可轻松实现不得不依赖于牙科技师的技能的高尺寸精度,因此,能够有效地形成患部适应性良好的金属框架,从这一点上看,预计将进一步普及(例如,参照专利文献2。)。On the other hand, recently, a method of measuring the three-dimensional shape of an affected part and forming a metal frame based on the obtained shape data has become widespread. This structure is called a dental CAD/CAM system. CAD (computer aided design) is a system that obtains the three-dimensional shape of an affected part through 3D scanning and digitizes it. Furthermore, CAM (computeraided design, computer-aided manufacturing) is a system that performs cutting processing on a workpiece based on numerical data generated by CAD, and cuts out a metal frame whose shape is suitable for the affected part. Since the dental CAD/CAM system that combines these systems can easily achieve high dimensional accuracy that has to rely on the skills of dental technicians, it is possible to efficiently form a metal frame that is well-adapted to the affected part. From this point of view, it is expected that Further spread (for example, refer to Patent Document 2.).
供牙科用CAD/CAM系统的被加工物通常被称为“坯材”。坯材除了需具备审美性、生物体适应性、化学稳定性、耐磨性这样的金属框架所需特性以外,还需具备切削性。切削性是可实施良好的切削加工的性质,通过使用切削性良好的坯材,从而根据由CAD生成的数值数据,能够利用CAM更有效地切出目标形状准确再现的金属框架。Workpieces for dental CAD/CAM systems are generally referred to as "blanks". In addition to the characteristics required for metal frames such as aesthetics, biocompatibility, chemical stability, and wear resistance, the billet must also have machinability. Machinability is a property that enables good machining, and by using a material with good machinability, it is possible to more efficiently cut out a metal frame that accurately reproduces the target shape using CAM based on numerical data generated by CAD.
专利文献1中记载的合金虽是适合于铸造的合金,但存在切削性差这一问题。若坯材的切削性低,则不能进行预期加工,且加工后的形状与所需形状之间会发生偏差。其结果是,增加因形状修正而需实施二次加工的时间,所以带来患部适应性低这样的不良结果。Although the alloy described in Patent Document 1 is suitable for casting, it has a problem of poor machinability. If the machinability of the material is low, desired processing cannot be performed, and deviations between the processed shape and the desired shape will occur. As a result, the time required for secondary processing due to shape correction is increased, which has the disadvantage of low adaptability to the affected part.
【现有技术文献】[Prior Art Literature]
【专利文献】【Patent Literature】
专利文献1:日本特开平11-1738号公报Patent Document 1: Japanese Patent Application Laid-Open No. 11-1738
专利文献2:日本特开2007-215854号公报Patent Document 2: Japanese Patent Laid-Open No. 2007-215854
发明内容Contents of the invention
本发明的目的在于提供切削性良好的牙科用的被切削加工用坯材、可制造上述被切削加工坯材的粉末冶金用金属粉末、陶材贴紧性良好的牙科用的烤瓷用金属框架、以及可靠性高的牙科用修补物。The object of the present invention is to provide a dental blank to be machined with good machinability, a metal powder for powder metallurgy capable of producing the above-mentioned machined blank, and a dental metal frame for porcelain with good adhesion to ceramic materials. , and dental restorations with high reliability.
上述目的是通过下述的本发明实现。The above objects are achieved by the present invention described below.
本发明的牙科用的被切削加工用坯材的特征在于,Co是主成分,以占质量比26%以上占质量比35%以下的比例含有Cr,以占质量比5%以上占质量比12%以下的比例含有Mo,以占质量比0.3%以上占质量比2.0%以下的比例含有Si,以占质量比0.09%以上占质量比0.5%以下的比例含有N,所述牙科用的被切削加工用坯材由金属粉末的烧结体构成。The dental material to be machined according to the present invention is characterized in that Co is the main component, and Cr is contained in a ratio of not less than 26% by mass and not more than 35% by mass, and is contained by a ratio of not less than 5% by mass and 12% by mass. % or less contains Mo, contains Si in a mass ratio of 0.3% or more and 2.0% or less in mass ratio, and contains N in a mass ratio of 0.09% or more and 0.5% or less. The blank for processing is composed of a sintered body of metal powder.
由此,可形成烧结体专有的结构,因此,可得到切削性良好的牙科用的被切削加工用坯材。Thereby, a structure unique to the sintered body can be formed, and therefore, a dental blank to be machined with good machinability can be obtained.
本发明的牙科用的被切削加工用坯材中,在该被切削加工用坯材的断面中,当将由表面起至深度为0.3mm的位置作为表层部,将由表面起至深度为5mm的位置作为内层部时,上述内层部的N浓度优选为上述表层部的N浓度的50%以上200%以下。In the dental material to be machined according to the present invention, in the cross section of the material to be machined, if the surface layer is defined as the surface portion from the surface to the depth of 0.3 mm, the position from the surface to the depth of 5 mm is In the case of an inner layer, the N concentration of the inner layer is preferably 50% or more and 200% or less of the N concentration of the surface layer.
由此,内层部与表层部的物理性能接近,在对牙科用的被切削加工用坯材实施切削加工时,可以抑制切削过程中切削性的变化。因此,切出的金属框架的尺寸精度难以降低。而且,能够抑制金属框架的机械特性的部分不相同。As a result, the physical properties of the inner layer portion and the surface layer portion are close, and when cutting a dental material to be machined, changes in machinability during cutting can be suppressed. Therefore, the dimensional accuracy of the cut out metal frame is difficult to decrease. Furthermore, the portion capable of suppressing the mechanical properties of the metal frame differs.
本发明的牙科用的被切削加工用坯材中,在该被切削加工用坯材的断面中,当将由表面起至深度为0.3mm的位置作为表层部,将由表面起至深度为5mm的位置作为内层部时,上述内层部的维氏硬度优选为上述表层部的维氏硬度的67%以上150%以下。In the dental material to be machined according to the present invention, in the cross section of the material to be machined, if the surface layer is defined as the surface portion from the surface to the depth of 0.3 mm, the position from the surface to the depth of 5 mm is In the case of an inner layer part, the Vickers hardness of the inner layer part is preferably 67% or more and 150% or less of the Vickers hardness of the surface layer part.
由此,内层部与表层部的硬度接近,在对牙科用的被切削加工用坯材实施切削加工时,可以抑制切削过程中切削性的变化。因此,切出的金属框架的尺寸精度难以降低。Accordingly, the hardness of the inner layer portion and the surface layer portion are close to each other, and it is possible to suppress a change in machinability during cutting when cutting a dental material to be machined. Therefore, the dimensional accuracy of the cut out metal frame is difficult to decrease.
在本发明的牙科用的被切削加工用坯材中,优选所述内层部的维氏硬度为200以上480以下。In the dental workpiece material of the present invention, it is preferable that the Vickers hardness of the inner layer part is 200 or more and 480 or less.
由此,能得到可制造对咬合力具有足够的耐变形性的金属框架的坯材。而且,由于切削阻力变得比较小,因此,能得到切削性良好且可有效地切出所需形状、尺寸的金属框架的坯材。Thereby, it is possible to obtain a material capable of producing a metal frame having sufficient deformation resistance against the occlusal force. Furthermore, since the cutting resistance becomes relatively small, it is possible to obtain a metal frame material which has good machinability and can efficiently cut out a desired shape and size.
在本发明的牙科用的被切削加工用坯材中,优选上述N的含有率相对上述Si的含有率的比例为0.1以上0.8以下。In the dental workpiece material of the present invention, it is preferable that the ratio of the above-mentioned N content to the above-mentioned Si content is 0.1 to 0.8.
由此,可以同时实现高机械特性和高切削性。即,通过添加一定量的Si,可提高切削性,另一方面,若Si的添加量过多,则有可能坯材的机械特性会降低。因此,当以上述范围内的比例添加N,则可在因添加了Si而获得的高切削性与因添加了N而获得的效果不会彼此相抵的情况下发挥作用,因此,可以协同改善切削性。而且,通过N固溶可抑制因Si固溶而导致的晶体结构的畸变,因此,可以防止机械特性的降低。此外,若添加Si,晶体结构会发生畸变,在这种状态下,因热膨胀和热收缩的行为而容易出现大的迟滞。若因热膨胀和热收缩的行为而出现大的迟滞,则坯材的热特性有可能会随时间而改变。对此,通过以上述比例添加N,可使N侵入晶体结构中并固溶,从而可抑制晶体结构的畸变。其结果是,可以抑制因热膨胀和热收缩的行为而出现的迟滞,实现坯材的热特性的稳定化。Thus, high mechanical properties and high machinability can be simultaneously achieved. That is, by adding a certain amount of Si, the machinability can be improved. On the other hand, if the added amount of Si is too large, there is a possibility that the mechanical properties of the material will be reduced. Therefore, when N is added at a ratio within the above range, the high machinability obtained by the addition of Si and the effect obtained by the addition of N will not cancel each other out, so that the machinability can be synergistically improved. sex. Furthermore, the solid solution of N can suppress the distortion of the crystal structure due to the solid solution of Si, and therefore, the reduction of mechanical properties can be prevented. In addition, if Si is added, the crystal structure is distorted, and in this state, a large hysteresis tends to occur due to the behavior of thermal expansion and thermal contraction. If large hysteresis occurs due to the behavior of thermal expansion and thermal contraction, the thermal properties of the billet may change over time. On the other hand, by adding N at the above-mentioned ratio, N can penetrate into the crystal structure and form a solid solution, thereby suppressing distortion of the crystal structure. As a result, hysteresis due to behavior of thermal expansion and thermal contraction can be suppressed, and the thermal properties of the billet can be stabilized.
本发明的牙科用的被切削加工用坯材中,优选所述Si中的一部分作为氧化硅而被含有,所述Si中的作为所述氧化硅而被含有的Si的比率是占质量比10%以上占质量比90%以下。In the dental material to be machined according to the present invention, it is preferable that a part of the Si is contained as silicon oxide, and the ratio of Si contained as the silicon oxide in the Si is 10% by mass. More than % accounts for less than 90% of the mass ratio.
由此,可带来高切削性、金属框架的高机械特性、陶材的高贴紧性这样的效果,另一方面,由于存在一定量的氧化硅,能够充分抑制该坯材中含有的Co、Cr、Mo这样的过渡金属元素的氧化物的含量。其结果是,使得牙科用修补物可实现更高的可靠性。Thus, the effects of high machinability, high mechanical properties of the metal frame, and high adhesion of ceramic materials can be brought about. On the other hand, due to the presence of a certain amount of silicon oxide, the Co contained in the material can be sufficiently suppressed. The content of oxides of transition metal elements such as , Cr, and Mo. As a result, a higher reliability of the dental prosthesis is achieved.
本发明的牙科用的被切削加工用坯材中,优选所述氧化硅在所述烧结体的晶界偏析。In the dental workpiece material of the present invention, it is preferable that the silicon oxide is segregated at the grain boundaries of the sintered body.
由此,能更可靠地抑制金属结晶的肥大化,从而得到可切出机械特性更良好的金属框架的坯材。而且,在晶界(grain boundary)偏析的氧化硅的析出物彼此能自然地保持适当的距离,因此,能够使坯材中的氧化硅的析出物更均匀地分散。结果,可得到更匀质的坯材。Thereby, enlargement of metal crystals can be more reliably suppressed, and a material from which a metal frame with better mechanical properties can be cut out can be obtained. Furthermore, since the precipitates of silicon oxide segregated at grain boundaries can naturally maintain an appropriate distance from each other, the precipitates of silicon oxide in the billet can be dispersed more uniformly. As a result, a more homogeneous billet can be obtained.
本发明的牙科用的被切削加工用坯材中,优选在通过使用了CuKα线的X射线衍射法得到的X射线衍射图谱中,当设起因于基于ICDD卡(国际衍射数据中心卡)确定的Co的峰中最高峰的高度为1时,起因于基于准衍射数据卡确定的Co3Mo的峰中最高峰的高度的比率为0.01以上0.5以下。In the dental material to be machined according to the present invention, it is preferable that in the X-ray diffraction pattern obtained by the X-ray diffraction method using CuKα ray, it is determined based on the ICDD card (International Center for Diffraction Data Card) When the height of the highest peak among the peaks of Co is 1, the ratio of the heights of the highest peak among the peaks of Co 3 Mo determined based on the quasi-diffraction data card is 0.01 to 0.5.
由此,可得到既可制造防止金属框架的硬度降低,难以因咬合力而变形的牙科用修补物,同时,又能抑制拉伸强度、耐力和伸长率的降低的坯材。Thereby, it is possible to obtain a raw material that prevents the decrease in hardness of the metal frame and prevents the dental prosthesis from being deformed due to occlusal force, and at the same time suppresses the decrease in tensile strength, endurance and elongation.
在本发明的牙科用的被切削加工用坯材中,优选所述牙科用的被切削加工用坯材的0.2%耐力为450MPa以上,伸长率为2%以上,杨氏模量为150GPa以上。In the dental material to be machined according to the present invention, the dental material to be machined preferably has a 0.2% proof strength of 450 MPa or more, an elongation of 2% or more, and a Young's modulus of 150 GPa or more. .
由此,能得到可制造耐久性卓越的金属框架的坯材。Thereby, a material from which a metal frame with excellent durability can be manufactured can be obtained.
本发明的粉末冶金用金属粉末的特征在于,Co是主成分,以占质量比26%以上占质量比35%以下的比例含有Cr,以占质量比5%以上占质量比12%以下的比例含有Mo,以占质量比0.3%以上占质量比2.0%以下的比例含有Si,以占质量比0.09%以上占质量比0.5%以下的比例含有N,所述粉末冶金用金属粉末用于制造牙科用的被切削加工用坯材。The metal powder for powder metallurgy of the present invention is characterized in that Co is the main component, and Cr is contained in a ratio of not less than 26% by mass and not more than 35% by mass, and a ratio of not less than 5% by mass and not more than 12% by mass Containing Mo, containing Si at a ratio of not less than 0.3% by mass and not more than 2.0% by mass, and containing N at a ratio of not less than 0.09% by mass and not more than 0.5% by mass, the metal powder for powder metallurgy is used to manufacture dental The billet used for machining.
由此,可得到能制造切削性卓越的牙科用的被切削加工用坯材的粉末冶金用金属粉末。Thereby, a metal powder for powder metallurgy capable of producing a material to be machined for dental use having excellent machinability can be obtained.
本发明的牙科用的烤瓷用金属框架的特征在于,Co是主成分,以占质量比26%以上占质量比35%以下的比例含有Cr,以占质量比5%以上占质量比12%以下的比例含有Mo,以占质量比0.3%以上占质量比2.0%以下的比例含有Si,以占质量比0.09%以上占质量比0.5%以下的比例含有N,所述牙科用的烤瓷用金属框架通过切削由金属粉末的烧结体构成的牙科用的被切削加工用坯材而得。The metal frame for dental porcelain of the present invention is characterized in that Co is the main component, Cr is contained in a ratio of 26% by mass to 35% by mass, and 5% by mass or more is 12% by mass. Mo is contained in the following proportions, Si is contained in a proportion of 0.3% to 2.0% by mass, and N is contained in a proportion of 0.09% to 0.5% by mass. The metal frame is obtained by cutting a dental blank to be processed which is composed of a sintered body of metal powder.
由此,可得到陶材贴紧性卓越的牙科用的烤瓷用金属框架。Thus, a dental metal frame for ceramics excellent in adhesion to ceramic materials can be obtained.
本发明的牙科用修补物的特征在于具有:本发明的牙科用的烤瓷用金属框架;以及陶材层,设置于所述牙科用的烤瓷用金属框架的表面。The dental prosthesis of the present invention is characterized by comprising: the dental metal frame for ceramics of the present invention; and a ceramic material layer provided on the surface of the dental metal frame for ceramics.
由此,能得到牙科用的烤瓷用金属框架与陶材层强力贴紧的可靠性高的牙科用修补物。Thus, a highly reliable dental prosthesis in which the dental metal frame for porcelain-for-porcelain and the ceramic material layer are strongly adhered to can be obtained.
在本发明的牙科用修补物中,优选所述陶材层包含氧化铝,所述牙科用修补物还具有位于所述牙科用的烤瓷用金属框架与所述陶材层之间的莫来石相。In the dental prosthesis of the present invention, it is preferable that the ceramic material layer contains alumina, and the dental prosthesis further has a mollusk between the dental ceramic metal frame and the ceramic material layer. Stone phase.
由此,可得到陶材层与金属框架通过莫来石相坚固地紧贴,陶材层难剥落的可靠性高的牙科用修补物。而且,通过形成莫来石相,在烤瓷处理时,可提高陶瓷材料对金属框架的润湿性。因此,从这一角度来看,陶材层的贴紧性也会提高。Thereby, the ceramic material layer and the metal frame are firmly adhered to each other through the mullite phase, and a highly reliable dental prosthesis in which the ceramic material layer is difficult to peel off can be obtained. Moreover, by forming the mullite phase, the wettability of the ceramic material to the metal frame can be improved during the porcelain firing process. Therefore, from this point of view, the adhesion of the ceramic material layer is also improved.
附图说明Description of drawings
图1是示出本发明的牙科用的被切削加工用坯材的实施方式的立体图。FIG. 1 is a perspective view showing an embodiment of a dental workpiece blank of the present invention.
图2是图1所示的牙科用的被切削加工用坯材的纵断面图。Fig. 2 is a longitudinal sectional view of the dental workpiece material shown in Fig. 1 .
图3是利用本发明的牙科用的被切削加工用坯材的电子束分析仪得到的Si组成图像的一例。Fig. 3 is an example of a Si composition image obtained by the electron beam analyzer of the dental workpiece blank of the present invention.
图4的(a)是本发明的牙科用的被切削加工用坯材的观察图像的一例,图4的(b)是原有技术的牙科用的被切削加工用坯材的观察图像的一例。Fig. 4(a) is an example of an observation image of a dental blank to be processed according to the present invention, and Fig. 4(b) is an example of an observation image of a conventional dental blank to be processed .
图5是用于说明测定本发明的牙科用的被切削加工用坯材的切削阻力的方法的图。Fig. 5 is a diagram for explaining a method of measuring the cutting resistance of the dental material to be machined according to the present invention.
图6的(a)、(b)是示出测定本发明的牙科用的被切削加工用坯材的切削阻力时,加工工具扫描坯材的轨迹的图。(a) and (b) of FIG. 6 are diagrams showing the trajectory of the machining tool scanning the blank when measuring the cutting resistance of the dental workpiece to be machined according to the present invention.
图7是示出对图1所示的坯材进行切出本发明的牙科用的烤瓷用金属框架的实施方式的加工后的状态的立体图。Fig. 7 is a perspective view showing a state after cutting out an embodiment of the dental porcelain metal frame of the present invention from the base material shown in Fig. 1 .
图8是图7的A-A线断面图。Fig. 8 is a sectional view taken along line A-A of Fig. 7 .
图9是示出本发明的牙科用的烤瓷用金属框架的实施方式的纵断面图。Fig. 9 is a longitudinal sectional view showing an embodiment of the metal frame for dental porcelain of the present invention.
图10是示出本发明的牙科用修补物的实施方式的纵断面图。Fig. 10 is a longitudinal sectional view showing an embodiment of the dental prosthesis of the present invention.
图11是示出各样品No.30~No.36的牙科用的被切削加工坯材中的N浓度与表层部和内层部的维氏硬度之间的关联性的坐标图。11 is a graph showing the correlation between the N concentration in the dental workpiece material of Sample No. 30 to No. 36 and the Vickers hardness of the surface layer part and the inner layer part.
具体实施方式Detailed ways
下面,根据附加图面所示的优选实施方式,对本发明的牙科用的被切削加工用坯材、粉末冶金用金属粉末、牙科用的烤瓷用金属框架及牙科用修补物进行详细说明。Next, the dental blank to be machined, the metal powder for powder metallurgy, the metal frame for dental porcelain, and the dental prosthesis of the present invention will be described in detail based on preferred embodiments shown in the attached drawings.
[牙科用的被切削加工用坯材][Bills for Dental Machining]
首先,对本发明的牙科用的被切削加工用坯材的实施方式进行说明。First, an embodiment of the dental workpiece blank of the present invention will be described.
图1是示出本发明的牙科用的被切削加工用坯材的实施方式的立体图,图2是图1所示的牙科用的被切削加工用坯材的纵断面图。FIG. 1 is a perspective view showing an embodiment of a dental blank to be machined according to the present invention, and FIG. 2 is a longitudinal sectional view of the dental blank to be machined shown in FIG. 1 .
图1所示的牙科用的被切削加工用坯材1(以下简称“坯材1”)是通过供以切削加工而用于切出所需形状的牙科金属配件的构件。如上所述,牙科用的被切削加工用坯材是用于牙科用CAD/CAM系统且包括通过CAM加工的“CAD/CAM坯材”、“牙科用研磨坯材(millblanks)”。牙科金属配件只要是可临时性或半永久性留置于口腔中的金属配件,则不受特别限定,但以下说明是对切出金属框架的情况进行的说明。A dental blank 1 to be machined (hereinafter referred to simply as "blank 1") shown in FIG. 1 is a member for cutting out a dental metal fitting of a desired shape by subjecting it to cutting. As described above, the dental workpiece to be machined is used in a dental CAD/CAM system and includes "CAD/CAM blanks" and "dental mill blanks" processed by CAM. The dental metal fittings are not particularly limited as long as they can be temporarily or semi-permanently placed in the oral cavity, but the following description is for the case of cutting out the metal frame.
图1和图2所示的坯材1形成为圆盘状、即高度比直径小的圆柱状,其上表面11和下表面12形成互相平行的平坦面。本发明的牙科用的被切削加工用坯材的形状不仅限于这样的圆盘状,可以是任何形状。例如,也可以是长方体、立方体、球形、多边形柱状等形状。The blank 1 shown in FIG. 1 and FIG. 2 is formed in a disk shape, that is, a cylinder with a height smaller than a diameter, and its upper surface 11 and lower surface 12 form flat surfaces parallel to each other. The shape of the dental workpiece to be machined according to the present invention is not limited to such a disc shape, but may be any shape. For example, shapes such as a rectangular parallelepiped, a cube, a sphere, and a polygonal column may also be used.
图1、2所示的坯材1形成为圆盘状、即高度比直径小的圆柱状,其上表面11和下表面12形成分别互相平行的平坦面。本发明的牙科用的被切削加工用坯材的形状不仅限于这样的圆盘状,可以是任何形状。例如,也可以是长方体、立方体、球形、多边形柱状等形状。The blank 1 shown in FIGS. 1 and 2 is formed in a disk shape, that is, a cylinder with a height smaller than a diameter, and its upper surface 11 and lower surface 12 form flat surfaces parallel to each other. The shape of the dental workpiece to be machined according to the present invention is not limited to such a disc shape, but may be any shape. For example, shapes such as a rectangular parallelepiped, a cube, a sphere, and a polygonal column may also be used.
这种坯材1由Co-Cr-Mo-Si-N类的合金构成。Such a material 1 is made of a Co-Cr-Mo-Si-N alloy.
具体而言,构成坯材1的合金是主成分为Co、以占质量比26%以上占质量比35%以下的比例含有Cr、以占质量比5%以上占质量比12%以下的比例含有Mo、以占质量比0.3%以上占质量比2.0%以下的比例含有Si、以占质量比0.09%以上占质量比0.5%以下的比例含有N的合金。Specifically, the alloy constituting the billet 1 is a main component of Co, containing Cr in a ratio of not less than 26% by mass and not more than 35% by mass, and containing Cr in a ratio of not less than 5% by mass and not more than 12% by mass. Mo, an alloy containing Si in a ratio of not less than 0.3% by mass and not more than 2.0% by mass, and containing N in a ratio of not less than 0.09% by mass and not more than 0.5% by mass.
由这种合金构成的坯材1具有生物体适应性、化学稳定性,同时也具有良好的切削性。因此,对坯材1进行切削加工并切出金属框架时,在切削屑顺利排出的同时,切削面的粗糙度也变得足够小,从而能够长时间地连续进行切削加工。而且,也能够将切削工具的缺损、磨损抑制在最小范围。其结果是,切削加工过程的切削量可达到预期,从而能够使切出的金属框架达到设计的尺寸、形状。The billet 1 made of this alloy has biocompatibility, chemical stability, and good machinability. Therefore, when cutting the blank 1 to cut out the metal frame, the cutting chips are smoothly discharged, and the roughness of the cut surface is sufficiently small, so that the cutting can be continuously performed for a long time. Furthermore, chipping and wear of the cutting tool can also be suppressed to a minimum. As a result, the cutting amount of the cutting process can reach the expected, so that the cut out metal frame can reach the designed size and shape.
而且,这种金属框架能够以较少不适感安装于患部,且能将患者的负担抑制到最小限度,同时可实现烤瓷时的高贴紧性和高审美性。In addition, this metal frame can be attached to the affected area with less discomfort, and can minimize the burden on the patient, while achieving high adhesion and high aesthetics during porcelain firing.
在这里,构成该合金的元素中,Co(钴)是构成坯材1的合金的主成分,会对坯材1的基本特性产生大的影响。Here, among the elements constituting the alloy, Co (cobalt) is a main component of the alloy constituting the material 1 and greatly affects the basic properties of the material 1 .
Co的含有率被设定为构成该合金的元素中最高,具体而言,优选为占质量比50%以上占质量比67.5%以下,更优选为占质量比55%以上占质量比67%以下。The content of Co is set to be the highest among the elements constituting the alloy. Specifically, it is preferably 50% by mass or more and 67.5% by mass or less, more preferably 55% by mass or more and 67% by mass or less. .
Cr(铬)主要起到提高坯材1的耐腐蚀性的作用。这可以考虑由于通过添加Cr,而在合金易于形成钝化膜(passivation film)(Cr2O3等),并增强化学稳定性。通过耐腐蚀性的改善,可望达到例如即便在与体液接触了的情况下,金属离子也难以溶出的效果。因此,由含有Cr的合金构成的坯材1堪称是可以切出生物体适应性更好的金属框架的坯材。而且,通过将Cr与Co和Mo、Si同时使用,从而可以提高金属框架的机械特性。Cr (chromium) mainly functions to improve the corrosion resistance of the billet 1 . This is considered to be because the addition of Cr facilitates the formation of a passivation film (Cr 2 O 3 , etc.) in the alloy and enhances the chemical stability. Improvement in corrosion resistance can be expected to prevent metal ions from being eluted, for example, even when it comes into contact with body fluids. Therefore, the material 1 made of the alloy containing Cr can be said to be a material from which a metal frame with better adaptability to the body can be cut out. Furthermore, by using Cr together with Co, Mo, and Si, the mechanical properties of the metal frame can be improved.
设定构成坯材1的合金中的Cr的含有率为占质量比26%以上占质量比35%以下。如果Cr的含有率低于上述下限值,则由坯材1切出的金属框架的耐腐蚀性会降低。因此,当金属框架长期与体液接触时,担心发生金属离子的溶出。另一方面,如果Cr的含有率高于上述上限值,则担心相对于Mo、Si的Cr的量相对过多,切削性下降。而且,Co、Mo、Si之间会失衡,机械特性会降低。The content of Cr in the alloy constituting the billet 1 is set to be 26% by mass or more and 35% by mass or less. If the content rate of Cr is less than the above-mentioned lower limit, the corrosion resistance of the metal frame cut out from the material 1 will fall. Therefore, there is a concern that elution of metal ions occurs when the metal frame is in contact with body fluids for a long period of time. On the other hand, if the content of Cr is higher than the above-mentioned upper limit, the amount of Cr relative to Mo and Si may be relatively large, and machinability may be reduced. In addition, Co, Mo, and Si are out of balance, and mechanical properties are degraded.
另外,Cr的含有率优选为占质量比27%以上占质量比34%以下,更优选为占质量比28%以上占质量比33%以下。In addition, the Cr content is preferably not less than 27% by mass and not more than 34% by mass, more preferably not less than 28% by mass and not more than 33% by mass.
Mo(钼)主要起到提高坯材1的耐腐蚀性的作用。即,添加Mo比添加Cr更能提高耐腐蚀性。这是考虑由于通过添加Mo,使得以Cr的氧化物为主要材料的钝化膜更致密。因此,添加有Mo的合金,其金属离子更难以溶出,从而有助于实现生物体适应性特别高的金属框架。Mo (molybdenum) mainly functions to improve the corrosion resistance of the billet 1 . That is, adding Mo improves corrosion resistance more than adding Cr. This is because the addition of Mo makes the passivation film mainly made of Cr oxide denser. Therefore, alloys to which Mo is added make it difficult for metal ions to elute, which contributes to the realization of a metal frame with particularly high biocompatibility.
构成坯材1的合金中的Mo的含有率为占质量比5%以上占质量比12%以下。如果Mo的含有率低于上述下限值,则担心由坯材1切出的金属框架的耐腐蚀性不充分。另一方面,如果Mo的含有率高于上述上限值,则担心相对于Cr和Si的Mo的量相对过多,切削性会下降。The content of Mo in the alloy constituting the material 1 is not less than 5% by mass and not more than 12% by mass. If the content rate of Mo is less than the above-mentioned lower limit, there is a concern that the corrosion resistance of the metal frame cut out from the material 1 may be insufficient. On the other hand, if the content of Mo is higher than the above-mentioned upper limit, the amount of Mo relative to Cr and Si may be relatively large, and the machinability may decrease.
另外,Mo的含有率优选为占质量比5.5%以上占质量比11%以下,更优选为占质量比6%以上占质量比9%以下。In addition, the content of Mo is preferably not less than 5.5% by mass and not more than 11% by mass, more preferably not less than 6% by mass and not more than 9% by mass.
此外,Si(硅)主要起到提高坯材1的切削性的作用。通过添加Si,坯材1中会生成由部分硅氧化而得的氧化硅。作为氧化硅,可例举有SiO、SiO2等。坯材1中若生成这种氧化硅,则金属结晶会在这个部位分裂。因此,在氧化硅周围,认为坯材1的构造局部会变得不连续。如果使用切削工具对这种状态的坯材1进行切削加工,则从切削工具的尖头产生的切削屑离开坯材1本体时,考虑氧化硅成为基点而易于分离。其结果是,切削阻力会降低,考虑坯材1的切削性会提高。In addition, Si (silicon) mainly functions to improve the machinability of the material 1 . By adding Si, silicon oxide obtained by partially oxidizing silicon is generated in the raw material 1 . As silicon oxide, SiO, SiO2 , etc. are mentioned. When such silicon oxide is generated in the material 1, the metal crystals will be split at this site. Therefore, it is considered that the structure of the material 1 becomes partially discontinuous around silicon oxide. When the billet 1 in this state is cut using a cutting tool, when chips generated from the tip of the cutting tool leave the body of the billet 1, silicon oxide is considered to be a base point and is likely to be separated. As a result, the cutting resistance is reduced, and the machinability of the material 1 is considered to be improved.
另一方面,Si也在提高由坯材1切出的金属框架的机械特性方面起作用。上述氧化硅在制造坯材1的过程中金属结晶成长时,可抑制金属结晶显著肥大。因此,添加了Si的合金中,金属结晶的粒径可抑制为较小,从而能进一步提高金属框架的机械特性。On the other hand, Si also plays a role in improving the mechanical properties of the metal frame cut out from the billet 1 . The above-mentioned silicon oxide suppresses the metal crystals from being significantly enlarged when the metal crystals grow in the process of manufacturing the billet 1 . Therefore, in the Si-added alloy, the grain size of the metal crystals can be suppressed to be small, and the mechanical properties of the metal frame can be further improved.
因此,通过添加Si,能够实现坯材1的切削性、由坯材1切出金属框架的机械特性这两者。Therefore, by adding Si, both the machinability of the raw material 1 and the mechanical properties of the metal frame cut out from the raw material 1 can be realized.
而且,通过添加Si,能够提高陶材对由坯材1切出的金属框架的贴紧。因此,设置陶材层使得其覆盖金属框架的表面时,可抑制陶材层的剥落,且可得到可靠性高的牙科用修补物。Furthermore, by adding Si, the adhesion of the ceramic material to the metal frame cut out from the blank 1 can be improved. Therefore, when the ceramic material layer is provided so as to cover the surface of the metal frame, peeling of the ceramic material layer can be suppressed, and a highly reliable dental prosthesis can be obtained.
而且,要得到上述效果,需将Si的含有率设定为占质量比0.3%以上占质量比2.0%以下。如果Si的含有率低于上述下限值,则氧化硅的量会减少,所以切削阻力将增大,坯材1的切削性将下降,同时,在制造坯材1时金属结晶容易变肥大,因此,由坯材1切出的金属框架的机械特性下降的可能性变高。而且,由于陶材对金属框架的贴紧性也变得不充分,因此,牙科用修补物易于发生陶材层剥落等不良情况。另一方面,如果Si的含有率超过上述上限值,则存在于坯材1中的氧化硅将会过多,易于产生氧化硅在空间上连续分布的区域。由于在该区域上,坯材1的构造会以一定的大小间不连续,因此,当外力施加于坯材1时该区域易于成为破坏的起点。因此,坯材1的机械特性会降低。Furthermore, in order to obtain the above effects, the content of Si needs to be set to 0.3% by mass or more and 2.0% by mass or less. If the content of Si is lower than the above-mentioned lower limit, the amount of silicon oxide will decrease, so the cutting resistance will increase, the machinability of the blank 1 will decrease, and at the same time, the metal crystals will easily become enlarged when the blank 1 is produced, Therefore, there is a high possibility that the mechanical properties of the metal frame cut out from the blank 1 will be degraded. Furthermore, since the adhesiveness of the ceramic material to the metal frame becomes insufficient, defects such as peeling of the ceramic material layer tend to occur in the dental prosthesis. On the other hand, if the content of Si exceeds the above-mentioned upper limit, too much silicon oxide will be present in the material 1, and regions where silicon oxide is spatially continuously distributed tend to occur. Since the structure of the blank 1 is discontinuous to a certain extent in this region, this region tends to become a starting point of damage when an external force is applied to the blank 1 . Therefore, the mechanical properties of the billet 1 are lowered.
另外,Si的含有率优选为占质量比0.5%以上占质量比1.0%以下,更优选为占质量比0.6%以上占质量比0.9%以下。In addition, the content of Si is preferably not less than 0.5% by mass and not more than 1.0% by mass, more preferably not less than 0.6% by mass and not more than 0.9% by mass.
而且,优选Si中的一部分以氧化硅的状态如上所述地存在,但其存在量中,相对于Si的总量,作为氧化硅而含有的Si的比率优选为占质量比10%以上占质量比90%以下,更优选为占质量比20%以上占质量比80%以下,进一步优选为占质量比30%以上占质量比70%以下,尤其优选为占质量比35%以上占质量比65%以下。通过将全部Si中的作为氧化硅而含有的Si的比率设定为上述范围内,从而可使坯材1在达到上述切削性、金属框架的机械特性、陶材的贴紧性等效果,另一方面,由于存在一定量的氧化硅,而能够充分抑制该坯材1所含有的Co、Cr、Mo等过渡金属元素的氧化物量。这也就是说,由于Si比Co、Cr和Mo更易于氧化,由Si夺走与这些过渡金属元素结合的氧而导致发生还原反应,因此,考虑Si的总量非氧化硅,等于是使过渡金属元素发生充分的还原反应。因此,通过将Si中作为氧化硅而含有的Si的比率设定在上述范围内,从而能够抑制坯材1中上述高切削性、金属框架的高机械特性、陶材的高贴紧性等效果受到Co、Cr或Mo的氧化物而阻碍。其结果是,可以实现可靠性更高的牙科用修补物。In addition, it is preferable that a part of Si exists in the state of silicon oxide as described above, but in the amount of Si, the ratio of Si contained as silicon oxide is preferably 10% by mass or more with respect to the total amount of Si. The ratio is less than 90%, more preferably more than 20% by mass and less than 80% by mass, more preferably more than 30% by mass and less than 70% by mass, especially preferably more than 35% by mass and 65% by mass %the following. By setting the ratio of Si contained as silicon oxide in the total Si within the above range, the raw material 1 can achieve the above-mentioned machinability, mechanical properties of the metal frame, and adhesion to ceramic materials. On the one hand, due to the presence of a certain amount of silicon oxide, the amount of oxides of transition metal elements such as Co, Cr, and Mo contained in the material 1 can be sufficiently suppressed. That is to say, since Si is easier to oxidize than Co, Cr, and Mo, Si takes away the oxygen combined with these transition metal elements to cause a reduction reaction. Therefore, considering that the total amount of Si is not silicon oxide, it is equivalent to making the transition Metal elements undergo a sufficient reduction reaction. Therefore, by setting the ratio of Si contained as silicon oxide in Si within the above-mentioned range, the above-mentioned effects of high machinability, high mechanical properties of the metal frame, and high adhesion of ceramic materials in the material 1 can be suppressed. Hindered by Co, Cr or Mo oxides. As a result, a more reliable dental prosthesis can be realized.
而且,通过将Si中作为氧化硅而含有的Si的比率设定在上述范围内,可赋予坯材1以合适的硬度。即,由于存在一定量的非氧化硅的Si,Co、Cr和Mo中的至少一种会与Si生成硬质的金属间化合物,其可提高坯材1的硬度。由于通过使坯材1的硬度增大,由坯材1切出的金属框架的硬度也相应增大,因此,包含该金属框架的牙科用修补物装到患部上后,很难因咬合力而变形,其将成为可靠性高的牙科用修补物。换言之,由于通过添加Si,使金属结晶的显著成长受到阻碍,从这个角度而言,坯材1的硬度呈下降趋势,但由于一部分Si生成金属间化合物,从而可抑制该硬度的显著降低,从而能够确保作为牙科用修补物的可靠性。Furthermore, by setting the ratio of Si contained as silicon oxide in Si within the above-mentioned range, it is possible to impart appropriate hardness to the material 1 . That is, due to the presence of a certain amount of Si other than silicon oxide, at least one of Co, Cr, and Mo forms a hard intermetallic compound with Si, which can increase the hardness of the billet 1 . Since the hardness of the blank 1 is increased, the hardness of the metal frame cut out from the blank 1 is also correspondingly increased. Therefore, after the dental prosthesis including the metal frame is installed on the affected part, it is difficult to damage it due to the occlusal force. deformed, it will become a highly reliable dental prosthesis. In other words, since the addition of Si inhibits the significant growth of metal crystals, the hardness of the material 1 tends to decrease from this point of view, but since a part of Si forms intermetallic compounds, this significant decrease in hardness can be suppressed, thereby Reliability as a dental prosthesis can be ensured.
作为这种金属间化合物,不受特别限定,可举出一例,如CoSi2、Cr3Si、MoSi2、Mo5Si3等。Such an intermetallic compound is not particularly limited, and examples include CoSi 2 , Cr 3 Si, MoSi 2 , Mo 5 Si 3 and the like.
另外,相对Si的总量,作为氧化硅而含有的Si的比率可通过重量法和ICP发射光谱法求得。In addition, the ratio of Si contained as silicon oxide to the total amount of Si can be obtained by a gravimetric method and an ICP emission spectrometry.
而且,若考虑金属间化合物的析出量,则相对于Mo的含有率,Si的含有率的比例(Si/Mo)优选为占质量比0.05以上0.2以下,更优选为0.08以上0.15以下。由此,能够在抑制坯材1的切削性显著降低的同时,得到能制造可靠性高的牙科用修补物的坯材1。Furthermore, considering the precipitation amount of intermetallic compounds, the ratio of the Si content (Si/Mo) to the Mo content is preferably a mass ratio of 0.05 to 0.2, and more preferably 0.08 to 0.15. Accordingly, it is possible to obtain a blank 1 capable of producing a highly reliable dental prosthesis while suppressing a significant decrease in the machinability of the blank 1 .
而且,氧化硅可以分布于任何位置,但优选以偏析于晶界(金属结晶之间的界面)的方式分布。通过使氧化硅偏析于这样的位置,从而可得到能够更可靠地抑制金属结晶的肥大化且能切出机械特性更良好的金属框架的坯材1。而且,偏析于晶界的氧化硅的析出物彼此自然而然地保持适当的距离,因此,可使坯材1中的氧化硅的析出物更均匀地分散。其结果是,可得到更匀质的坯材1。Furthermore, silicon oxide may be distributed anywhere, but is preferably distributed so as to be segregated at grain boundaries (interfaces between metal crystals). By segregating silicon oxide in such a position, it is possible to obtain a raw material 1 that can more reliably suppress the enlargement of metal crystals and cut out a metal frame with better mechanical properties. In addition, since the precipitates of silicon oxide segregated at the grain boundaries naturally keep an appropriate distance from each other, the precipitates of silicon oxide in the material 1 can be dispersed more uniformly. As a result, a more homogeneous material 1 can be obtained.
这种坯材1即便在从其中切出了多个金属框架的情况下,也有利于最大限度地减少金属框架之间的特性的个体差异。Such a blank material 1 is advantageous in minimizing individual differences in properties between metal frames even when a plurality of metal frames are cut out therefrom.
而且,对于偏析的氧化硅的析出物,可以通过定性分析中的表面分析,鉴定其大小、分布等。具体而言,在使用电子束分析仪(EPMA)得到的Si组成图像中,Si在偏析区域的平均直径优选为0.1μm以上10μm以下,更优选为0.3μm以上8μm以下。如果Si在偏析区域的平均直径为上述范围内,则氧化硅的析出物的大小在实现上述各种效果的过程中是最优的。即,如果Si在偏析区域的平均直径低于上述下限值,则氧化硅的析出物不会偏析于足够的大小,有可能无法充分达到上述各种效果,另一方面,如果Si在偏析区域的平均直径超过上述上限值,则有可能坯材1的机械特性会降低。Furthermore, the size, distribution, etc. of segregated silicon oxide precipitates can be identified by surface analysis in qualitative analysis. Specifically, in the Si composition image obtained using an electron beam analyzer (EPMA), the average diameter of Si in the segregation region is preferably 0.1 μm to 10 μm, more preferably 0.3 μm to 8 μm. If the average diameter of Si in the segregation region is within the above-mentioned range, the size of the precipitates of silicon oxide is optimal in achieving the above-mentioned various effects. That is, if the average diameter of Si in the segregation region is lower than the above-mentioned lower limit value, the precipitates of silicon oxide will not segregate in a sufficient size, and the above-mentioned various effects may not be sufficiently achieved. On the other hand, if Si is in the segregation region If the average diameter exceeds the above-mentioned upper limit, the mechanical properties of the billet 1 may decrease.
另外,在Si组成图像中,Si在偏析区域的平均直径可以作为与Si所偏析区域的面积具有相同面积的圆的直径(投影面积等效圆直径)的平均值来求得。而且,Si在偏析区域的平均直径是对100个以上Si所偏析的区域测定平均值而求得的。In addition, in the Si composition image, the average diameter of Si in the segregated region can be obtained as an average value of the diameters of circles having the same area as the area of the Si segregated region (projected area equivalent circle diameter). In addition, the average diameter of Si in segregated regions is obtained by measuring the average value of 100 or more regions in which Si is segregated.
图3是利用本发明的牙科用的被切削加工用坯材的电子束分析仪得到的Si组成图像的一例。Fig. 3 is an example of a Si composition image obtained by the electron beam analyzer of the dental workpiece blank of the present invention.
从该组成图像可以看出,本发明的牙科用的被切削加工用坯材中,可观察到Si局部凝集,同时,该凝集物(图3的淡色部分)是分散的。考虑这表明了氧化硅在晶界偏析。As can be seen from this compositional image, in the dental material to be machined according to the present invention, Si is locally aggregated and the aggregates (light-colored portion in FIG. 3 ) are dispersed. Consider this to indicate the segregation of silicon oxide at grain boundaries.
而且,坯材1包括:主要由Co构成的第一相(phase)、主要由Co3Mo构成的第二相。其中,通过含有第二相,可与包含上述Si的金属间化合物同样地赋予金属框架以适当硬度,因此,从提高牙科用修补物的可靠性的角度来看,可得到有用的坯材1。另一方面,若过量含有第二相,由于其易于偏析,则可能导致拉伸强度、耐力、伸长率等机械特性下降。Furthermore, the material 1 includes a first phase (phase) mainly composed of Co and a second phase mainly composed of Co 3 Mo. Among them, by containing the second phase, it is possible to impart appropriate hardness to the metal frame similarly to the above-mentioned intermetallic compound containing Si, so that a useful material 1 can be obtained from the viewpoint of improving the reliability of the dental prosthesis. On the other hand, if the second phase is contained in excess, mechanical properties such as tensile strength, strength, and elongation may decrease because it is likely to segregate.
因此,从上述角度出发,优选以适当比率含有第一相和第二相。具体而言,当通过使用CuKα线的X射线衍射法对坯材1进行晶体结构分析,并将起因于Co的峰中最高峰的高度定为1时,起因于Co3Mo的峰中最高峰的高度优选为0.01以上0.5以下,更优选为0.02以上0.4以下。Therefore, from the above viewpoint, it is preferable to contain the first phase and the second phase at an appropriate ratio. Specifically, when the crystal structure of material 1 was analyzed by X-ray diffraction using CuKα rays, and the height of the highest peak among the peaks due to Co was set to 1, the highest peak among the peaks due to Co3Mo The height of is preferably not less than 0.01 and not more than 0.5, and more preferably not less than 0.02 and not more than 0.4.
而且,若设Co的上述峰高度为1时的Co3Mo的上述峰高度的比率低于上述下限值,则坯材1中Co3Mo对Co的比率会下降,因此,金属框架的硬度会降低,担心使牙科用修补物易于因咬合力而变形。另一方面,若Co3Mo的上述峰高度的比率超过上述上限值,则Co3Mo会过量存在,因此,Co3Mo变得易于偏析,担心使拉伸强度和耐力降低,同时使伸长率也下降。Moreover, if the ratio of the above-mentioned peak height of Co 3 Mo when the above-mentioned peak height of Co is 1 is lower than the above-mentioned lower limit value, the ratio of Co 3 Mo to Co in the material 1 will decrease, so the hardness of the metal frame will be reduced. will be lowered, worrying about making the dental prosthesis susceptible to deformation due to occlusal forces. On the other hand, if the ratio of the above-mentioned peak heights of Co 3 Mo exceeds the above-mentioned upper limit, Co 3 Mo will be present in excess, and therefore Co 3 Mo will be likely to segregate, which may lower the tensile strength and resistance, and cause the tensile strength to decrease. Length also decreased.
另外,CuKα线通常是能量为8.048keV的特征X射线。In addition, CuKα rays are generally characteristic X-rays with an energy of 8.048keV.
而且,在确定起因于Co的峰时,需基于ICDD(The International Centre forDiffraction Data,国际衍射数据中心)卡的Co的数据库进行确定。同样地,在确定起因于Co3Mo的峰时,需基于ICDD卡的Co3Mo的数据库确定。In addition, when specifying the peak derived from Co, it is necessary to specify based on the Co database of the ICDD (The International Center for Diffraction Data, International Center for Diffraction Data) card. Similarly, when determining the peak originating from Co 3 Mo, it is necessary to determine based on the Co 3 Mo database of the ICDD card.
而且,在坯材1中,Co3Mo的存在比率优选为占质量比0.01%以上占质量比10%以下,更优选为占质量比0.05%以上占质量比5%以下。由此,可得到具有适当硬度、拉伸强度、耐力和伸长率的金属框架,从而得到很难因咬合力而变形的牙科用修补物。Furthermore, in the raw material 1, the abundance ratio of Co 3 Mo is preferably not less than 0.01% by mass and not more than 10% by mass, more preferably not less than 0.05% by mass and not more than 5% by mass. As a result, a metal frame having appropriate hardness, tensile strength, durability, and elongation can be obtained, thereby obtaining a dental prosthesis that is hardly deformed by occlusal force.
另外,这些存在比率可通过由晶体结构分析的结果对Co3Mo的存在比率进行定量化来求得。In addition, these abundance ratios can be obtained by quantifying the abundance ratio of Co 3 Mo from the results of crystal structure analysis.
而且,N(氮)的主要作用是提高坯材1的机械特性。由于N是奥氏体化元素,因此,在促进坯材1的晶体结构的奥氏体化、抑制坯材1的硬度增加的同时,还起提高韧性的作用。Also, the main role of N (nitrogen) is to improve the mechanical properties of the billet 1 . Since N is an austenitizing element, it promotes the austenitization of the crystal structure of the material 1 and suppresses an increase in the hardness of the material 1, and also plays a role of improving toughness.
而且,通过含有N,由金属粉末的烧结体构成的坯材1中,枝晶相的生成会受到抑制,枝晶相的含有率会变得非常小。从这样的角度来看,可以抑制坯材1的硬度上升,同时也可以提高韧性。Furthermore, by containing N, in the material 1 made of a sintered body of metal powder, the formation of a dendrite phase is suppressed, and the content of the dendrite phase becomes very small. From such a point of view, the increase in hardness of the material 1 can be suppressed, and the toughness can also be improved.
而且,如上所述,含有N的坯材1,既具有适当的硬度,韧性又高,且会成为枝晶相的含有率小的坯材。因此,这样的坯材1切削性高,并可有效地切出尺寸精度高的金属框架。Furthermore, as described above, the material 1 containing N has appropriate hardness and high toughness, and is a material with a low dendrite phase content. Therefore, such a material 1 has high machinability and can efficiently cut out a metal frame with high dimensional accuracy.
在这里,枝晶相是成长为树枝状的晶体组织,大量含有这样的枝晶相的坯材1,其切削性会降低。因此,使枝晶相的含有率减小,在提高坯材1的切削性上是有效的。具体而言,使用扫描型电子显微镜观察坯材1,所得的观察图像中枝晶相所占的面积比优选为20%以下,更优选为10%以下。满足这种条件的坯材1,其机械特性、切削性特别优异。Here, the dendrite phase is a crystal structure that grows into a dendrite, and the material 1 containing a large amount of such a dendrite phase will have lower machinability. Therefore, reducing the content of the dendrite phase is effective in improving the machinability of the material 1 . Specifically, the area ratio of the dendrite phase in the observation image obtained by observing the material 1 using a scanning electron microscope is preferably 20% or less, more preferably 10% or less. The material 1 satisfying these conditions is particularly excellent in mechanical properties and machinability.
而且,如上所述,坯材1由金属粉末的烧结体构成。金属粉末各粒子的体积非常小,冷却速度高,冷却的均匀性也高。因此,在这样的由金属粉末的烧结体构成的坯材1中,枝晶相的生成会受到抑制。另一方面,若使用铸造等传统方法,由于将熔融金属浇入形成了坯材形状的模具中,因此,需被冷却的体积非常大。因此,冷却速度低,冷却的均匀性也低。其结果是,通过这种方法制造的坯材中会生成大量的枝晶相。Furthermore, as described above, the blank 1 is composed of a sintered body of metal powder. The volume of each particle of the metal powder is very small, the cooling rate is high, and the uniformity of cooling is also high. Therefore, in the green material 1 composed of such a sintered body of metal powder, the generation of dendrite phase is suppressed. On the other hand, with conventional methods such as casting, the volume to be cooled is very large because molten metal is poured into a mold that forms the shape of the billet. Therefore, the cooling rate is low, and the uniformity of cooling is also low. As a result, a large number of dendrite phases are formed in billets produced by this method.
另外,上述面积比是作为枝晶相所占面积相对于观察图像面积的比例算出的,观察图像的一个边设定为50μm以上1000μm以下程度。In addition, the above-mentioned area ratio is calculated as a ratio of the area occupied by the dendrite phase to the area of the observation image, and one side of the observation image is set to be approximately 50 μm or more and 1000 μm or less.
为得到上述效果,需将N的含有率设定为占质量比0.09%以上占质量比0.5以下。若N的含有率低于上述下限值,则坯材1的晶体结构的奥氏体化会不充分,因此,坯材1的硬度会非常高,韧性也会降低。因此,坯材1的切削性和机械特性会降低。这考虑由于坯材1中除了奥氏体相(γ相)以外,还析出大量密排六方(hcp)结构(ε相)。另一方面,若N的含有率高于上述上限值,则在大量生成各种氮化物的同时,会成为难以烧结的组成。因此,因此,坯材1的烧结密度会下降,机械特性也会降低。作为生成的氮化物,可举例如Cr2N等。若这种氮化物析出,则硬度会增大,韧性还是会降低。In order to obtain the above-mentioned effects, the content of N needs to be set to not less than 0.09% by mass and not more than 0.5% by mass. If the N content is lower than the above lower limit, the crystal structure of the material 1 will not be sufficiently austenitized, so the hardness of the material 1 will be very high, and the toughness will also decrease. Therefore, the machinability and mechanical properties of the raw material 1 are lowered. This is considered to be due to the precipitation of a large amount of hexagonal close-packed (hcp) structure (ε phase) in addition to the austenite phase (γ phase) in the material 1 . On the other hand, if the content of N is higher than the above-mentioned upper limit, a large amount of various nitrides will be formed, and the composition will be difficult to sinter. Therefore, the sintered density of the green material 1 is lowered, and the mechanical properties are also lowered. Examples of nitrides to be formed include Cr 2 N and the like. If such nitrides are precipitated, the hardness will increase, but the toughness will still decrease.
另外,N的含有率优选为占质量比0.12%以上占质量比0.4%以下,更优选为占质量比0.14%以上占质量比0.25%以下,尤其优选为占质量比0.15%以上占质量比0.22%以下。In addition, the content of N is preferably not less than 0.12% by mass and not more than 0.4% by mass, more preferably not less than 0.14% by mass and not more than 0.25% by mass, especially preferably not less than 0.15% by mass and not more than 0.22% by mass. %the following.
尤其是在占质量比0.15%以上占质量比0.22%以下的范围内,可以观察到奥氏体相特别占优势,硬度显著降低,韧性明显提高。当将这时的坯材1供以通过使用CrKα线的X射线衍射法进行的晶体结构分析,可观察到起因于奥氏体相的主峰非常强,另一方面,起因于密排六方结构的峰和其它峰均为主峰高度的5%以下。由此可知奥氏体相占优势。Especially in the range of more than 0.15% by mass and less than 0.22% by mass, it can be observed that the austenite phase is particularly dominant, the hardness is significantly reduced, and the toughness is obviously improved. When the billet 1 at this time was subjected to crystal structure analysis by X-ray diffraction method using CrKα ray, it was observed that the main peak originating from the austenite phase was very strong, and on the other hand, the main peak originating from the hexagonal close-packed structure was observed. Both peaks and other peaks are less than 5% of the height of the main peak. It can be seen that the austenite phase is dominant.
另一方面,N的含有率对Si的含有率的比例(N/Si)优选为质量比0.1以上0.8以下,更优选为0.2以上0.6以下。由此,可同时实现高机械特性和高切削性。即,通过添加一定量的Si,如上所述切削性会增强,另一方面,若Si的添加量过多,担心坯材1的机械特性会降低。因此,若以上述范围内的比例添加N,则可在因添加了Si而获得的高切削性与因添加了N而获得的上述效果不会彼此相抵的情况下发挥作用,因此,可以协同改善切削性。这考虑由于相对于Si与Co等金属元素生成置换型固溶体,N与Co等金属元素生成侵入型固溶体,因此,彼此可共存。而且,Si固溶而导致的晶体结构的畸变会因N固溶而受到抑制。因此,可防止机械特性的降低。On the other hand, the ratio of the N content to the Si content (N/Si) is preferably a mass ratio of 0.1 to 0.8, more preferably 0.2 to 0.6. Accordingly, both high mechanical properties and high machinability can be achieved. That is, by adding a certain amount of Si, the machinability is enhanced as described above. On the other hand, if the amount of Si added is too large, there is a concern that the mechanical properties of the material 1 may be reduced. Therefore, if N is added at a ratio within the above range, the high machinability obtained by the addition of Si and the above effect obtained by the addition of N will work without canceling each other out, so synergistic improvement can be achieved. machinability. This is considered because metal elements such as Si and Co form substitution-type solid solutions, and metal elements such as N and Co form intrusion-type solid solutions, so that they can coexist with each other. Furthermore, the distortion of the crystal structure caused by the solid solution of Si is suppressed by the solid solution of N. Therefore, reduction in mechanical characteristics can be prevented.
而且,若添加Si,如上所述晶体结构会产生畸变,在这种状态下因热膨胀和热收缩的行为而易于出现大的迟滞。若存在因热膨胀和热收缩的行为而出现大的迟滞,担心坯材1的热特性会随时间而改变。Furthermore, if Si is added, the crystal structure is distorted as described above, and a large hysteresis tends to occur due to the behavior of thermal expansion and thermal contraction in this state. If there is a large hysteresis due to the behavior of thermal expansion and thermal contraction, there is a concern that the thermal properties of the billet 1 will change over time.
对此,通过以上述比例添加N,由于N侵入晶体结构中,晶体结构的畸变受到抑制。其结果是,可抑制因热膨胀和热收缩的行为而出现的迟滞,从而可实现坯材1的热特性的稳定。In contrast, by adding N in the above ratio, distortion of the crystal structure is suppressed due to N intrusion into the crystal structure. As a result, hysteresis due to behavior of thermal expansion and thermal contraction can be suppressed, so that the thermal characteristics of the billet 1 can be stabilized.
从以上所述,通过适度添加Si和N,从而可在提高坯材1的切削性的同时,分别实现机械特性的稳定和热特性的稳定。From the above, by appropriately adding Si and N, the machinability of the material 1 can be improved, and the stability of the mechanical properties and the stability of the thermal properties can be achieved, respectively.
另外,若N的含有率对Si的含有率的比例低于上述下限值,则不能充分抑制晶体结构的畸变,担心韧性等下降。另一方面,若高于上述上限值,则担心会形成难以烧结的组成,坯材1的烧结密度会降低,机械特性也会降低。In addition, if the ratio of the N content to the Si content is below the above lower limit, the distortion of the crystal structure cannot be sufficiently suppressed, and there is a concern that the toughness and the like may decrease. On the other hand, if it exceeds the above-mentioned upper limit, there is a possibility that a composition that is difficult to sinter will be formed, the sintered density of the green material 1 will decrease, and the mechanical properties will also decrease.
另外,构成坯材1的合金,除了含有上述各元素以外,还可含有C(碳)。通过添加C,能增强坯材1的硬度、拉伸强度,同时也增强切削性。切削性增强的详细原因尚不明确,但碳化物的生成可减小切削阻力是其中的一个原因。而且,由于C与Co等金属元素生成侵入型固溶体,所以即使添加C也基本不会导致韧性的降低(脆性增加)。因此,可在保持一定的韧性的同时,提高切削性。In addition, the alloy constituting the material 1 may contain C (carbon) in addition to the above elements. By adding C, the hardness and tensile strength of the billet 1 can be enhanced, and machinability can also be enhanced. The detailed reason for the enhanced machinability is not clear, but the reduction of cutting resistance due to the formation of carbides is one of the reasons. Furthermore, since C forms an intrusive solid solution with metal elements such as Co, even if C is added, the decrease in toughness (increase in brittleness) hardly occurs. Therefore, machinability can be improved while maintaining a certain toughness.
构成坯材1的合金中的C的含有率不受特别限定,但优选为占质量比1.5%以下,更优选为占质量比0.7%以下。若C的含有率超过上述上限值,则担心坯材1的脆性会增大,机械特性也会降低。The content of C in the alloy constituting the material 1 is not particularly limited, but is preferably 1.5% by mass or less, more preferably 0.7% by mass or less. When the content of C exceeds the above-mentioned upper limit, the brittleness of the material 1 may increase and the mechanical properties may also decrease.
而且,添加量的下限值不受特别限定,但为了能充分发挥上述效果,优选将下限值设定为占质量比0.05%程度。In addition, the lower limit of the added amount is not particularly limited, but it is preferable to set the lower limit to about 0.05% by mass in order to fully exhibit the above effects.
而且,C的含有率优选为Si的含有率的0.02倍以上0.5倍以下程度,更优选为0.05倍以上0.3倍以下程度。通过将C对Si的比率设定在上述范围内,可将氧化硅、碳化物对坯材1的机械特性造成的不利影响控制在最小限度,同时,在切削性的提高上发挥协同作用。因此,能得到切削性特别优良的坯材1。Furthermore, the C content is preferably about 0.02 to 0.5 times the Si content, more preferably about 0.05 to 0.3 times. By setting the ratio of C to Si within the above range, the adverse effects of silicon oxide and carbide on the mechanical properties of the material 1 can be minimized, and at the same time, a synergistic effect can be exerted on the improvement of machinability. Therefore, a material 1 having particularly excellent machinability can be obtained.
而且,N的含有率优选为C的含有率的0.3倍以上10倍以下程度,更优选为2倍以上8倍以下程度。通过将N对C的比率设定在上述范围内,尤其能够使因添加C而提高的坯材1的切削性,以及因添加N而提高的坯材1的机械特性同时实现。Furthermore, the content of N is preferably about 0.3 to 10 times the content of C, more preferably about 2 to 8 times. By setting the ratio of N to C within the above range, the machinability of the raw material 1 enhanced by the addition of C and the mechanical properties of the raw material 1 improved by the addition of N can be realized at the same time.
此外,构成坯材1的合金中,除上述各种元素以外,在不阻碍上述效果的范围内允许有意加入微量的添加物、在制造时也允许混入不可避免地会产生的杂质。这种情况下,添加物、杂质的合计含有率优选为占质量比1%以下,更优选为占质量比0.5%以下,进一步优选为占质量比0.2%以下。作为这种添加物元素、杂质元素,可例举Li、B、N、O、Na、Mg、Al、P、S、Mn、K、Ca、Sc、Ti、V、Co、Zn、Ga、Ge、Y、Pd、Ag、In、Sn、Sb、Hf、Ta、W、Os、Ir、Pt、Au、Bi等。In addition, in the alloy constituting the material 1, in addition to the above-mentioned various elements, it is allowed to add a small amount of additives intentionally within the range that does not hinder the above-mentioned effects, and it is also allowed to mix unavoidable impurities during production. In this case, the total content of additives and impurities is preferably 1% by mass or less, more preferably 0.5% by mass or less, even more preferably 0.2% by mass or less. Examples of such additive elements and impurity elements include Li, B, N, O, Na, Mg, Al, P, S, Mn, K, Ca, Sc, Ti, V, Co, Zn, Ga, Ge , Y, Pd, Ag, In, Sn, Sb, Hf, Ta, W, Os, Ir, Pt, Au, Bi, etc.
另一方面,构成坯材1的合金优选实际上不包含Ni(镍)。在原有的坯材中,为了确保塑性加工性,大多含有一定量的Ni,但其有时被作为金属过敏诱发物质对待,也是担心有可能对生物体产生影响的元素。在构成坯材1的合金中,除了制造时不可避免会混入的Ni,不添加作为构成元素的Ni。因此,由本发明涉及的坯材1切出的金属框架很难产生金属过敏,生物体适应性特别高。另外,在本发明中,由于添加有适量的Si,从而即便没有添加Ni,也能实现具有足够切削性的坯材1。而且,考虑到不可避免地会混入的情况,Ni的含有率优选为占质量比0.05%以下,更优选为占质量比0.03%以下。On the other hand, the alloy constituting the material 1 preferably does not substantially contain Ni (nickel). Conventional billets often contain a certain amount of Ni in order to ensure plastic workability, but Ni is sometimes treated as a metal allergy-inducing substance, and it is also an element that is concerned that it may affect living organisms. In the alloy constituting the billet 1 , Ni is not added as a constituent element other than Ni which is unavoidably mixed during manufacture. Therefore, the metal frame cut out from the material 1 according to the present invention is less prone to metal allergy, and has particularly high biocompatibility. In addition, in the present invention, since an appropriate amount of Si is added, the material 1 having sufficient machinability can be realized even without adding Ni. Furthermore, in consideration of unavoidable contamination, the Ni content is preferably 0.05% by mass or less, more preferably 0.03% by mass or less.
而且,在构成坯材1的合金中,上述各元素的剩余部分是Co。如上所述,Co的含有率被设定为在构成坯材1的合金中所含元素中最高。Furthermore, in the alloy constituting the billet 1, the balance of the above-mentioned elements is Co. As described above, the content of Co is set to be the highest among the elements contained in the alloy constituting the material 1 .
另外,构成坯材1的合金的各构成元素及组成比,可通过例如JIS G1257(2000)中规定的铁及钢-原子吸光法、JIS G 1258(2007)中规定的铁及钢-ICP发光分析法、JIS G1253(2002)中规定的铁及钢-火花发光分析法、JIS G 1256(1997)中规定的铁及钢-X射线荧光分析法、JIS G 1211~G 1237中规定的重量法滴定法吸光光度法等来指定。具体而言,例如:SPECTRO公司制造的固体发光分光分析装置(火花发光分析装置)、型号:SPECTROLAB、类型:LAVMBO8A。In addition, each constituent element and the composition ratio of the alloy constituting the material 1 can be emitted by, for example, iron and steel-atomic absorption method specified in JIS G1257 (2000) and iron and steel-ICP specified in JIS G 1258 (2007). Analytical method, iron and steel specified in JIS G1253 (2002) - spark emission analysis method, iron and steel specified in JIS G 1256 (1997) - X-ray fluorescence analysis method, gravimetric method specified in JIS G 1211 to G 1237 Titration, absorptiometry, etc. to specify. Specifically, for example: solid-state luminescence spectroscopic analyzer (spark luminescence analyzer) manufactured by SPECTRO, model: SPECTROLAB, type: LAVMBO8A.
此外,JIS G 1211~G 1237如下所述。In addition, JIS G 1211 to G 1237 are as follows.
JIS G 1211(2011) 铁及钢-碳定量法JIS G 1211(2011) Iron and Steel-Carbon Quantitative Method
JIS G 1212(1997) 铁及钢-硅定量方法JIS G 1212(1997) Iron and Steel-Silicon Quantitative Method
JIS G 1213(2001) 铁及钢中的锰定量方法JIS G 1213(2001) Quantitative method of manganese in iron and steel
JIS G 1214(1998) 铁及钢-磷定量方法JIS G 1214(1998) Iron and Steel - Quantitative Method of Phosphorus
JIS G 1215(2010) 铁及钢-硫磺定量方法JIS G 1215(2010) Iron and Steel-Sulfur Quantitative Method
JIS G 1216(1997) 铁及钢-镍定量方法JIS G 1216(1997) Iron and Steel - Nickel Quantitative Method
JIS G 1217(2005) 铁及钢-铬定量方法JIS G 1217(2005) Iron and Steel - Chromium Quantitative Method
JIS G 1218(1999) 铁及钢-钼定量方法JIS G 1218(1999) Iron and Steel - Molybdenum Quantitative Method
JIS G 1219(1997) 铁及钢-铜定量方法JIS G 1219(1997) Iron and steel-copper quantitative method
JIS G 1220(1994) 铁及钢-钨定量方法JIS G 1220(1994) Iron and Steel - Tungsten Quantitative Method
JIS G 1221(1998) 铁及钢-钒定量方法JIS G 1221(1998) Iron and Steel - Quantitative Method of Vanadium
JIS G 1222(1999) 铁及钢-钴定量方法JIS G 1222(1999) Iron and Steel - Cobalt Quantitative Method
JIS G 1223(1997) 铁及钢-钛定量方法JIS G 1223(1997) Quantitative method for iron and steel-titanium
JIS G 1224(2001) 铁及钢中的铝定量方法JIS G 1224(2001) Quantitative method of aluminum in iron and steel
JIS G 1225(2006) 铁及钢-砷定量方法JIS G 1225(2006) Iron and Steel - Quantitative Method for Arsenic
JIS G 1226(1994) 铁及钢-锡定量方法JIS G 1226(1994) Iron and Steel - Tin Quantitative Method
JIS G 1227(1999) 铁及钢中的硼定量方法JIS G 1227(1999) Quantitative method of boron in iron and steel
JIS G 1228(2006) 铁及钢-氮定量方法JIS G 1228(2006) Iron and Steel - Nitrogen Quantitative Method
JIS G 1229(1994) 钢-铅定量方法JIS G 1229(1994) Steel-lead quantitative method
JIS G 1232(1980) 钢中的锆定量方法JIS G 1232(1980) Quantitative method for zirconium in steel
JIS G 1233(1994) 钢-硒定量方法JIS G 1233(1994) Steel-selenium quantitative method
JIS G 1234(1981) 钢中的碲定量方法JIS G 1234(1981) Quantitative method for tellurium in steel
JIS G 1235(1981) 铁及钢中的锑定量方法JIS G 1235(1981) Quantitative method of antimony in iron and steel
JIS G 1236(1992) 钢中的钽定量方法JIS G 1236(1992) Quantitative method of tantalum in steel
JIS G 1237(1997) 铁及钢-铌定量方法JIS G 1237(1997) Iron and Steel - Niobium Quantitative Method
而且,在C(碳)和S(硫)的指定时,尤其也可以采用JIS G 1211(2011)中规定的氧流量燃烧(高频感应加热炉燃烧)-红外线吸收法。具体而言,例如LECO公司制造的CS-200碳硫分析仪。Furthermore, when specifying C (carbon) and S (sulfur), the oxygen flow combustion (combustion in a high-frequency induction heating furnace)-infrared ray absorption method stipulated in JIS G 1211 (2011) can also be used. Specifically, for example, CS-200 carbon-sulfur analyzer manufactured by LECO Corporation.
而且,在N(氮)和O(氧)的指定时,尤其也可采用JIS G 1228(2006)中规定的铁和钢的氮定量法、JIS Z 2613(2006)中规定的金属材料的氧定量法。具体而言,例如LECO公司制造的氧/氮分析装置、TC-300/EF-300。In addition, when specifying N (nitrogen) and O (oxygen), the nitrogen quantitative method for iron and steel specified in JIS G 1228 (2006) and the oxygen content of metal materials specified in JIS Z 2613 (2006) can also be used. quantitative method. Specifically, for example, an oxygen/nitrogen analyzer manufactured by LECO Corporation, TC-300/EF-300.
而且,如图1所示的坯材1由金属粉末的烧结体构成,即由粉末冶金法制造而得。这种坯材1与例如由铸造法制造的坯材(熔炼材)相比,具有优良的硬度、拉伸强度、耐力、伸长率等机械特性。这是由于通过粉末冶金法制造的坯材1是使用急冷而得的金属粉末制造而成(体积小,易于急冷),与铸造法等相比很难发生金属结晶的显著晶粒成长,因此,考虑是基于很难生成肥大的金属结晶这一烧结体独有的特征。而且,由于使用粉末冶金法,组成易于匀质,因此,Si、氧化硅的分布也容易均匀。因此,可得到切削性也均匀的坯材1。Furthermore, the blank 1 shown in FIG. 1 is composed of a sintered body of metal powder, that is, manufactured by powder metallurgy. Such a billet 1 has superior mechanical properties such as hardness, tensile strength, endurance, elongation, etc., compared with, for example, a billet (cast material) produced by a casting method. This is because the billet 1 produced by the powder metallurgy method is manufactured using rapidly cooled metal powder (small in size, easy to rapidly cooled), and it is difficult to produce significant grain growth of metal crystals compared with casting methods, etc. Therefore, The consideration is based on the unique characteristic of sintered body that it is difficult to generate hypertrophic metal crystals. Furthermore, since the powder metallurgy method is used, the composition is easily homogeneous, and therefore the distribution of Si and silicon oxide is also easy to be uniform. Therefore, the raw material 1 which is also uniform in machinability can be obtained.
作为用于坯材1的制造的金属粉末(本发明的粉末冶金用金属粉末),可使用上述由合金构成的粉末。其平均粒径优选为3μm以上100μm以下,更优选为4μm以上80μm以下,进一步优选为5μm以上60μm以下。通过使用这种粒径的金属粉末,可以制造高密度、机械特性高且切削性卓越的坯材1。As the metal powder (the metal powder for powder metallurgy of the present invention) used in the production of the billet 1 , the powder composed of the alloy described above can be used. The average particle diameter is preferably 3 μm to 100 μm, more preferably 4 μm to 80 μm, and still more preferably 5 μm to 60 μm. By using a metal powder having such a particle size, a billet 1 having a high density, high mechanical properties, and excellent machinability can be produced.
另外,在通过激光衍射法得到的粒度分布中,平均粒径是作为以质量标准计算从小径侧的累积量为50%时的粒径求得的。In addition, in the particle size distribution obtained by the laser diffraction method, the average particle diameter is calculated as the particle diameter when the cumulative amount from the diameter side is 50% calculated on a mass basis.
而且,在金属粉末的平均粒径低于上述下限值的情况下,由于粉末冶金的成型性下降,因此,有可能坯材1的密度会降低,金属框架的机械特性会下降。另一方面,在金属粉末的平均粒径超过上述上限值的情况下,由于粉末冶金中金属粉末的填充性降低,因此,担心坯材1的密度仍然会降低,金属框架的机械特性会降低。而且,担心组成的均匀性会受到损害,坯材1的切削性会降低。Furthermore, when the average particle size of the metal powder is less than the above-mentioned lower limit, the formability of powder metallurgy decreases, so the density of the material 1 may decrease, and the mechanical properties of the metal frame may decrease. On the other hand, when the average particle size of the metal powder exceeds the above upper limit, since the filling property of the metal powder in powder metallurgy is lowered, there is a concern that the density of the blank 1 will be lowered and the mechanical properties of the metal frame will be lowered. . Furthermore, there is a concern that the uniformity of the composition may be impaired, and the machinability of the billet 1 may be reduced.
而且,金属粉末的粒度分布优选尽可能狭窄。具体而言,若金属粉末的平均粒径在上述范围内,则最大粒径优选为200μm以下,更优选为150μm以下。通过将金属粉末的最大粒径控制在上述范围内,可使得金属粉末的粒度分布更狭窄,从而能够进一步提高坯材1的机械特性和切削性。Also, the particle size distribution of the metal powder is preferably as narrow as possible. Specifically, if the average particle diameter of the metal powder is within the above range, the maximum particle diameter is preferably 200 μm or less, more preferably 150 μm or less. By controlling the maximum particle size of the metal powder within the above range, the particle size distribution of the metal powder can be made narrower, so that the mechanical properties and machinability of the blank 1 can be further improved.
另外,上述最大粒径是指在通过激光衍射法得到的粒度分布中,以质量标准计算从小径侧的累积量达99.9%时的粒径。In addition, the above-mentioned maximum particle diameter refers to the particle diameter at which the cumulative amount from the diameter side reaches 99.9% by mass standard calculation in the particle size distribution obtained by the laser diffraction method.
而且,当金属粉末颗粒的短径为PS[μm],长径为PL[μm]时,由PS/PL定义的宽高比的平均值优选为0.4以上1以下程度,更优选为0.7以上1以下程度。这种宽高比的金属粉末由于其形状比较接近于球形,因此,能提高压粉成型时的填充率。其结果是,可得到机械特性、切削性高的坯材1。Furthermore, when the short axis of the metal powder particles is PS [μm] and the long axis is PL [μm], the average value of the aspect ratio defined by PS/PL is preferably from 0.4 to 1, more preferably from 0.7 to 1 the following degree. Metal powders with such an aspect ratio can increase the filling rate during powder compaction because their shapes are closer to spherical. As a result, a material 1 having high mechanical properties and machinability can be obtained.
另外,上述长径是指颗粒的投影像中可获得的最大长度,上述短径是与该最大长度垂直方向的最大长度。而且,宽高比的平均值是作为100个以上金属粉末颗粒的测定值的平均值来求得的。In addition, the above-mentioned major axis means the maximum length obtained in the projected image of the particles, and the above-mentioned short axis means the maximum length in the direction perpendicular to the maximum length. In addition, the average value of aspect ratio was calculated|required as the average value of the measured value of 100 or more metal powder particles.
另一方面,在坯材1的断面中,当结晶组织的长径为CL,短径为CS时,由CS/CL定义的宽高比的平均值优选为0.4以上1以下程度,更优选为0.5以上1以下程度。由于这种宽高比的结晶组织各向异性小,因此,有助于实现可制造无论力的施加方向如何,均显示出良好的耐力等机械特性的金属框架的坯材1。即,由这种坯材1切出的金属框架,无论以何种姿势使用,均具有良好的耐破折性,因此,不限定其在口腔中的使用位置,是很有用的。换言之,利用这样的坯材1,能够制造无论采用何种金属框架的切出方法,均显示出良好的机械特性的金属框架。On the other hand, in the cross section of the material 1, when the major axis of the crystal structure is CL and the minor axis is CS, the average value of the aspect ratio defined by CS/CL is preferably about 0.4 to 1, more preferably 0.5 or more and 1 or less. Since the anisotropy of the crystalline structure of such an aspect ratio is small, it contributes to the realization of the raw material 1 of a metal frame that can exhibit good mechanical properties such as endurance regardless of the direction of force application. That is, the metal frame cut out from such a blank 1 has good fracture resistance no matter what posture it is used in, so it is useful without limiting its use position in the oral cavity. In other words, using such a material 1 , it is possible to manufacture a metal frame that exhibits good mechanical properties regardless of the cutting method of the metal frame.
另外,上述长径是坯材1的断面的观察图像中一个结晶组织所能取得的最大长度,上述短径是与该最大长度垂直方向的最大长度。而且,宽高比的平均值是作为100个以上结晶组织的测定值的平均值来求得的。In addition, the above-mentioned major axis is the maximum length that can be obtained by one crystal structure in the observed image of the cross section of the billet 1, and the above-mentioned short axis is the maximum length in the direction perpendicular to the maximum length. In addition, the average value of the aspect ratio is calculated|required as the average value of the measured value of 100 or more crystal structures.
而且,优选坯材1在其内部具有微小独立的空孔。通过具有这种空孔,坯材1会成为切削性特别优异的坯材。这是因为由于存在独立的空孔,可抑制坯材1的机械特性下降,同时,该空孔成为起点而使得切削加工时产生的切削屑特别容易离开坯材1的本体,从而可取得切削阻力大大减少的效果。Furthermore, it is preferable that the blank 1 has fine independent pores inside it. By having such voids, the material 1 becomes a material particularly excellent in machinability. This is because the existence of independent voids can suppress the degradation of the mechanical properties of the blank 1. At the same time, the voids serve as the starting point, making it easier for chips generated during cutting to leave the body of the blank 1, thereby achieving cutting resistance. greatly reduced effect.
而且,通过使坯材1具有空孔,由坯材1切出的金属框架也就具有表面开口的空孔。在对金属框架烤瓷时,能使陶材的构成材料进入这种空孔中。因此,有助于提高金属框架与陶材之间的贴紧性。其结果是,当设置陶材层以覆盖金属框架的表面时,可得到能抑制陶材层的剥落,且可靠性高的牙科用修补物。Furthermore, by making the blank 1 have voids, the metal frame cut out from the blank 1 also has voids that are open on the surface. When ceramicing the metal frame, the constituent material of the pottery can be made to enter the voids. Therefore, it contributes to improving the adhesion between the metal frame and the ceramic material. As a result, when the ceramic layer is provided to cover the surface of the metal frame, peeling of the ceramic layer can be suppressed and a highly reliable dental prosthesis can be obtained.
空孔的平均直径优选为0.1μm以上10μm以下,更优选为0.3μm以上8μm以下。若空孔的平均直径在上述范围内,则可得到具有更高切削性的坯材1。即,若空孔的平均直径低于上述下限值,则担心无法充分提高切削性,另一方面,若空孔的平均直径超过上述上限值,则担心坯材1的机械特性会降低。The average diameter of the pores is preferably not less than 0.1 μm and not more than 10 μm, more preferably not less than 0.3 μm and not more than 8 μm. If the average diameter of the pores is within the above range, the material 1 having higher machinability can be obtained. That is, if the average diameter of the pores is less than the above lower limit, the machinability may not be sufficiently improved. On the other hand, if the average diameter of the pores exceeds the above upper limit, the mechanical properties of the material 1 may be reduced.
另外,在扫描型电子显微镜图像中,空孔的平均直径可以作为具有与空孔面积相同面积的圆的直径(投影面积的等效圆直径)的平均值来求得。而且,空孔的平均直径可作为100个以上空孔的测定值的平均值来求得。In addition, in the scanning electron microscope image, the average diameter of the pores can be obtained as an average value of the diameters of circles having the same area as the area of the pores (circle-equivalent diameter of the projected area). In addition, the average diameter of pores can be obtained as an average value of measured values of 100 or more pores.
而且,在坯材1的观察图像中,空孔所占的面积比优选为0.001%以上1%以下,更优选为0.005%以上0.5%以下。若空孔所占面积比在上述范围内,则可同时使坯材1具有更优异的机械特性和切削性。Furthermore, in the observed image of the material 1 , the area ratio occupied by voids is preferably from 0.001% to 1%, more preferably from 0.005% to 0.5%. If the area ratio of the pores is within the above range, the material 1 can have more excellent mechanical properties and machinability at the same time.
另外,该面积比是作为空孔相对于观察图像面积所占的面积比例而算出的,观察图像的一个边可设定为50μm以上1000μm以下程度。In addition, the area ratio is calculated as the area ratio of the voids to the area of the observation image, and one side of the observation image can be set to approximately 50 μm or more and 1000 μm or less.
图4的(a)是本发明的牙科用的被切削加工用坯材的观察图像的一例,图4的(b)是原有技术的牙科用的被切削加工用坯材的观察图像的一例。Fig. 4(a) is an example of an observation image of a dental blank to be processed according to the present invention, and Fig. 4(b) is an example of an observation image of a conventional dental blank to be processed .
图4的(a)所示的观察图像中可观察到存在基本上均匀分散的空孔,另一方面,图4的(b)所示的观察图像中可捕获到树枝状组织(枝晶相)。In the observation image shown in (a) of FIG. 4 , the presence of substantially uniformly dispersed voids can be observed. On the other hand, in the observation image shown in (b) of FIG. 4 , a dendritic structure (dendritic phase ).
而且,坯材1的维氏硬度优选为200以上480以下,更优选为240以上380以下。这种硬度的坯材1可制造即便对咬合力也具有足够的耐变形性的金属框架。而且,这种硬度的坯材1切削阻力比较小,因而切削性优异,将成为可有效地切出所需形状、尺寸的金属框架的坯材。Furthermore, the Vickers hardness of the material 1 is preferably not less than 200 and not more than 480, more preferably not less than 240 and not more than 380. A blank material 1 of this hardness can produce a metal frame having sufficient deformation resistance even against a occlusal force. Furthermore, the material 1 with such hardness has relatively low cutting resistance, and therefore has excellent machinability, and it will become a material from which a metal frame of a desired shape and size can be effectively cut out.
另外,坯材1的维氏硬度根据JIS Z 2244(2009)中规定的试验方法进行测定。In addition, the Vickers hardness of the material 1 was measured according to the test method prescribed|regulated by JIS Z 2244 (2009).
而且,坯材1的拉伸强度优选为520MPa以上,更优选为600MPa以上1500MPa以下。这种拉伸强度的坯材1将成为可制造耐久性优异的金属框架的坯材。而且,切削性也优异。Furthermore, the tensile strength of the material 1 is preferably 520 MPa or more, more preferably 600 MPa or more and 1500 MPa or less. The material 1 having such a tensile strength becomes a material from which a metal frame excellent in durability can be produced. Moreover, machinability is also excellent.
同样地,坯材1的0.2%耐力优选为450MPa以上,更优选为500MPa以上1200MPa以下。这种0.2%耐力的坯材1将成为可制造耐久性优异的金属框架的坯材。而且,切削性也优异。Similarly, the 0.2% proof strength of the material 1 is preferably 450 MPa or more, more preferably 500 MPa or more and 1200 MPa or less. Such a 0.2% proof material 1 will be a material from which a metal frame excellent in durability can be manufactured. Moreover, machinability is also excellent.
这些拉伸强度和0.2%耐力,根据JIS Z 2241(2011)中规定的试验方法进行测定。These tensile strengths and 0.2% proof strength were measured in accordance with the test method specified in JIS Z 2241 (2011).
而且,坯材1的伸长率优选为2%以上50%以下,更优选为10%以上45%以下。由于具有这种伸长率的坯材1很难发生缺损、开裂,因此,将成为切削性优异的坯材。Furthermore, the elongation of the material 1 is preferably not less than 2% and not more than 50%, more preferably not less than 10% and not more than 45%. Since the material 1 having such an elongation is less prone to chipping and cracking, it becomes a material having excellent machinability.
坯材1的伸长率(破断伸长率)根据JIS Z 2241(2011)中规定的试验方法进行测定。The elongation (elongation at break) of the material 1 was measured in accordance with the test method specified in JIS Z 2241 (2011).
而且,坯材1的杨氏模量优选为150GPa以上,更优选为170GPa以上300GPa以下。由于具有这种杨氏模量的坯材1变得难以变形,因此,可进行高尺寸精度的切削加工,同时可以实现难以因咬合力而变形的金属框架。而且,切削性也优异。Furthermore, the Young's modulus of the material 1 is preferably 150 GPa or more, more preferably 170 GPa or more and 300 GPa or less. Since the material 1 having such a Young's modulus becomes difficult to deform, cutting with high dimensional accuracy is possible, and at the same time, a metal frame that is hardly deformed by the occlusal force can be realized. Moreover, machinability is also excellent.
而且,坯材1的疲劳强度优选为250MPa以上,更优选为350MPa以上,进一步优选为500MPa以上1000MPa以下。具有这种疲劳强度的坯材1例如即便在口腔内与体液接触的状态下,在反复载荷作用的环境下使用,也能成为能够得到可抑制疲劳裂纹等的发生,并可长期体现其功能的金属框架的坯材。Furthermore, the fatigue strength of the material 1 is preferably 250 MPa or more, more preferably 350 MPa or more, and still more preferably 500 MPa or more and 1000 MPa or less. The material 1 having such a fatigue strength can be used in an environment where fatigue cracks and the like can be suppressed and can exhibit its function for a long period of time even if it is used in an environment where it is in contact with body fluids in the oral cavity, for example. Billet of metal frame.
另外,坯材1的疲劳强度根据JIS T 0309(2009)中规定的试验方法进行测定。假定相当于反复应力的载荷的施加波形为正弦波,应力比(最小应力/最大应力)为0.1。而且,假定重复频率为30Hz,重复次数为1×107次。In addition, the fatigue strength of the material 1 was measured according to the test method prescribed|regulated by JIS T 0309 (2009). Assuming that the applied waveform of the load corresponding to the repeated stress is a sine wave, the stress ratio (minimum stress/maximum stress) is 0.1. Also, assume that the repetition frequency is 30 Hz and the number of repetitions is 1×10 7 times.
而且,如上所述,这种坯材1由于切削阻力小,是切削性良好的坯材。Furthermore, as described above, such a material 1 is a material having good machinability due to its low cutting resistance.
也就是说,与和用于坯材1的制造的金属粉末相同组成的熔炼材的切削阻力相比,坯材1的切削阻力小。切削阻力小有助于将切削时加工工具振动的振幅控制在小范围内。因此,对坯材1实施切削加工时,能够容易且准确地切出所需形状,因此,能够制造尺寸精度高的金属框架。That is, the cutting resistance of the billet 1 is smaller than the cutting resistance of the molten material having the same composition as the metal powder used in the manufacture of the billet 1 . The small cutting resistance helps to control the vibration amplitude of the machining tool within a small range during cutting. Therefore, when the blank 1 is cut, a desired shape can be easily and accurately cut out, and therefore a metal frame with high dimensional accuracy can be manufactured.
具体而言,坯材1的切削阻力优选为300N以下,更优选为250N以下,进一步优选为200N以下。能以这种较小的切削阻力加工的坯材1,切削性高,可进行加工精度高的加工。Specifically, the cutting resistance of the material 1 is preferably 300N or less, more preferably 250N or less, even more preferably 200N or less. The material 1 that can be processed with such a small cutting resistance has high machinability and can be processed with high processing accuracy.
另外,坯材1的切削阻力可使用例如三成分切削测力仪来测定。In addition, the cutting resistance of the material 1 can be measured using, for example, a three-component cutting force gauge.
图5是用于说明测定坯材1的切削阻力的方法的图。FIG. 5 is a diagram for explaining a method of measuring the cutting resistance of the material 1 .
测定坯材1的切削阻力时,首先,如图5所示,需在加工装置的台(stage)74上载置三成分切削测力仪7。接着,将坯材1固定于三成分切削测力仪7的测定部71上。将使用螺丝的夹具72用于固定,螺丝紧固力矩为30kN。在这种状态下,使用加工工具73对坯材1进行切削加工。然后,可采用由三成分切削测力仪7在加工中测量的三方向的成分(x成分、y成分和z成分)的切削阻力中的最大值作为坯材1的切削阻力。而且,湿法加工中的切削阻力是使用切削液进行加工时的切削阻力。When measuring the cutting resistance of the material 1 , first, as shown in FIG. 5 , it is necessary to place a three-component cutting force gauge 7 on a stage 74 of the processing device. Next, the blank 1 is fixed to the measuring portion 71 of the three-component cutting force gauge 7 . A jig 72 using screws was used for fixing, and the screw tightening torque was 30 kN. In this state, the blank 1 is cut using the machining tool 73 . Then, the maximum value among the cutting resistances of three-directional components (x component, y component, and z component) measured by the three-component cutting force gauge 7 during machining can be adopted as the cutting resistance of the billet 1 . Furthermore, the cutting resistance in wet machining is the cutting resistance when machining is performed using a cutting fluid.
图6是示出测定坯材1的切削阻力时,相对于坯材1扫描加工工具73的轨迹TR的图。测定坯材1的切削阻力时,只要通过沿着坯材1的外形形状的轨迹TR来进行加工工具73的扫描即可。例如,当坯材1的外形形状为圆形时,如图6的(a)所示,只要通过如描绘圆形轨迹TR那样来进行加工工具73的扫描即可,当坯材1的外形形状为四角形时,如图6的(b)所示,只要通过如描绘四角形的轨迹TR那样来进行加工工具73的扫描即可。FIG. 6 is a diagram showing a trajectory TR of the machining tool 73 scanned with respect to the material 1 when measuring the cutting resistance of the material 1 . When measuring the cutting resistance of the material 1 , it is only necessary to scan the machining tool 73 along the trajectory TR of the outer shape of the material 1 . For example, when the outer shape of the blank 1 is circular, as shown in (a) of FIG. In the case of a square, as shown in (b) of FIG. 6 , it is only necessary to scan the processing tool 73 by drawing a quadrangular trajectory TR.
而且,作为用于坯材1的制造的金属粉末,可例举通过如下方法制造的金属粉末:雾化法(例如,水雾化法、气雾化法、高速旋转水流雾化法等)、还原法、羰基法、粉碎法等各种粉末化法。Furthermore, as the metal powder used in the production of the billet 1, metal powder produced by an atomization method (for example, a water atomization method, a gas atomization method, a high-speed rotary water flow atomization method, etc.), Various powdering methods such as reduction method, carbonyl method, pulverization method, etc.
其中,优选使用通过雾化法制造的坯材,更优选使用通过水雾化法或高速旋转水流雾化法制造的坯材。雾化法是通过使熔融金属(金属熔液)与高速喷射的流体(液体或气体)碰撞,在将熔融金属微粉化的同时进行冷却,从而制造金属粉末的方法。通过利用这种雾化法制造金属粉末,可有效地制造极其微小的粉末。而且,所得粉末的颗粒形状由于表面张力的作用而接近于球形。因此,在用粉末冶金法将金属粉末成型时,可得到填充率高的成型体。其结果是,可得到机械特性优异的坯材1。Among them, the material produced by the atomization method is preferably used, and the material produced by the water atomization method or the high-speed rotary water atomization method is more preferably used. The atomization method is a method of producing metal powder by colliding molten metal (melt metal) with a fluid (liquid or gas) sprayed at a high speed, cooling the molten metal while micronizing it. By producing metal powders using this atomization method, extremely fine powders can be produced efficiently. Moreover, the particle shape of the obtained powder is close to spherical due to the effect of surface tension. Therefore, when metal powder is molded by powder metallurgy, a molded body with a high filling rate can be obtained. As a result, a material 1 excellent in mechanical properties can be obtained.
另外,作为雾化法,在使用水雾化法的情况下,对熔融金属喷射的水(以下,称为“雾化水”)的压力不受特别限定,但优选为75MPa以上120MPa以下(750kgf/cm2以上1200kgf/cm2以下)程度,更优选为90MPa以上120MPa以下(900kgf/cm2以上1200kgf/cm2以下)程度。In addition, as the atomization method, in the case of using the water atomization method, the pressure of the water sprayed on the molten metal (hereinafter referred to as "atomized water") is not particularly limited, but is preferably 75 MPa or more and 120 MPa or less (750 kgf /cm 2 to 1200 kgf/cm 2 ), more preferably 90 MPa to 120 MPa (900 kgf/cm 2 to 1200 kgf/cm 2 ).
而且,雾化水的水温不受特别限定,但优选为1℃以上20℃以下程度。Furthermore, the water temperature of the atomized water is not particularly limited, but is preferably about 1°C to 20°C.
而且,雾化水大多在熔融金属的下落路径上具有顶点,并以外径向下方逐渐减小的这种圆锥状喷射。这种情况下,由雾化水形成的圆锥的顶角θ优选为10°以上40°以下程度,更优选为15°以上35°以下程度。由此,能够可靠地制造出上述组成的金属粉末。In addition, the atomized water often has an apex on the falling path of the molten metal, and is sprayed in a conical shape such that the outer diameter gradually decreases downward. In this case, the apex angle θ of the cone formed by the atomized water is preferably about 10° to 40°, and more preferably about 15° to 35°. Thereby, the metal powder of the said composition can be manufactured reliably.
而且,利用水雾化法(尤其是高速旋转水流雾化法),可以特别快速地冷却熔融金属。因此,可得到机械特性和切削性优异,且均质的坯材1。Furthermore, the molten metal can be cooled particularly rapidly by means of water atomization, especially high-speed rotary water atomization. Therefore, a homogeneous material 1 having excellent mechanical properties and machinability can be obtained.
而且,使用雾化法冷却熔融金属时的冷却速度优选为1×104℃/s以上,更优选为1×105℃/s以上。通过这样的急速冷却,可得到金属结晶的粒径特别小的金属粉末。Furthermore, the cooling rate when cooling the molten metal using the atomization method is preferably 1×104°C/s or higher, more preferably 1×105°C/s or higher. Through such rapid cooling, metal powder having a particularly small particle size of metal crystals can be obtained.
此外,在将原材料熔融而得到熔融金属时,假定坯材1的构成材料的熔点为Tm时,优选将原材料的熔融温度设定为Tm+50℃以上Tm+300℃以下程度,更优选设定为Tm+100℃以上Tm+200℃以下程度。由此,在使熔融金属与流体碰撞而进行微粉化时,易于控制合金的生成使其稳定。即,可抑制结晶组织的肥大化,同时又易于生成纯度高(含氧量少)的合金。因此,能够制造特别适合于坯材1的制造的金属粉末。In addition, when the raw material is melted to obtain molten metal, assuming that the melting point of the constituent material of the billet 1 is Tm, it is preferable to set the melting temperature of the raw material to about Tm+50°C or higher and Tm+300°C lower, more preferably set to It is about Tm+100°C or higher and Tm+200°C or lower. This makes it easy to control and stabilize the generation of alloys when the molten metal is collided with a fluid to be pulverized. That is, while suppressing the enlargement of the crystal structure, it is easy to produce an alloy with high purity (low oxygen content). Therefore, it is possible to produce a metal powder particularly suitable for production of the billet 1 .
利用各种成型法将以这种方式得到的金属粉末成型,从而得到成型体。作为成型方法,可例举如:加压成型法、挤出成型法、射出成型法等。The metal powder thus obtained is molded by various molding methods to obtain a molded body. As a molding method, a press molding method, an extrusion molding method, an injection molding method, etc. are mentioned, for example.
然后,通过对所得的成型体进行脱脂和烧制,可得到烧结体(坯材1)。烧成温度可根据合金组成适当设定,作为一个例子,如可设定为900℃以上1400℃以下程度。Then, by degreasing and firing the obtained molded body, a sintered body (blank 1) can be obtained. The firing temperature can be appropriately set according to the alloy composition, and as an example, it can be set at about 900°C to 1400°C.
而且,对于这样得到的烧结体,也可以进一步实施HIP处理(热等静压处理)等。由此,能够实现烧结体的更高密度,从而得到机械特性更优异的坯材1。Furthermore, the sintered body obtained in this way may be further subjected to HIP treatment (hot isostatic pressing treatment) or the like. As a result, a higher density of the sintered body can be realized, and the green material 1 with better mechanical properties can be obtained.
作为HIP处理的条件,例如,温度为850℃以上1200℃以下,时间为1小时以上10小时以下程度。The conditions for the HIP treatment are, for example, a temperature of 850° C. to 1200° C., and a time of about 1 hour to 10 hours.
而且,加压力优选为50MPa以上,更优选为100MPa以上。Furthermore, the applied pressure is preferably 50 MPa or more, more preferably 100 MPa or more.
另外,坯材1由从粉末制造时就在金属材料中固溶有N,并使用该粉末制得的烧结体构成。因此,在坯材1中,可使N基本均匀地分布,并可使物理性能也大致相同。因此,当由上述坯材1切出多个金属框架时,可以使各金属框架的特性一致,从而抑制个体差异。In addition, the material 1 is composed of a sintered body obtained by solid-dissolving N in a metal material from the time of powder production, and using the powder. Therefore, in the material 1, N can be distributed substantially uniformly, and physical properties can also be made substantially the same. Therefore, when a plurality of metal frames are cut out from the above-mentioned raw material 1, the properties of the respective metal frames can be made uniform and individual differences can be suppressed.
具体而言,例如,当坯材1的厚度为10mm以上时,将沿着坯材1的厚度方向的断面中,由表面至深度0.3mm的位置作为表层部,由表面至深度5mm的位置作为内层部。Specifically, for example, when the thickness of the blank 1 is 10 mm or more, in the section along the thickness direction of the blank 1, the position from the surface to a depth of 0.3 mm is defined as the surface layer, and the position from the surface to a depth of 5 mm is defined as the surface layer portion. inner part.
这种情况下,优选内层部的N的浓度为表层部的N的浓度的50%以上200%以下,更优选为60%以上175%以下,进一步优选为75%以上150%以下。若内层部的N的浓度对于上述下限值,或高于上述上限值,则由于内层部和表层部的物理性能不同,对坯材1进行切削加工时,担心切削过程中切削性会改变。因此,有可能切出的金属框架的尺寸精度会降低。而且,金属框架的机械特性也可能会有部分不同。In this case, the N concentration in the inner layer is preferably 50% to 200% of the N concentration in the surface layer, more preferably 60% to 175%, and even more preferably 75% to 150%. If the concentration of N in the inner layer is below the above-mentioned lower limit or higher than the above-mentioned upper limit, then due to the difference in physical properties between the inner layer and the surface layer, when cutting the billet 1, there is concern about machinability during cutting. will change. Therefore, there is a possibility that the dimensional accuracy of the cut out metal frame will be reduced. Also, the mechanical properties of the metal frame may also be partially different.
另外,内层部和表层部的N的浓度可以基于利用电子束分析仪(EPMA)的N的定量分析来求得。这种情况下,通过从坯材1的表面至内部进行线分析,可得到坯材1的厚度方向的N的浓度分布,因此,能够有效地求出上述内层部和表层部的N的浓度。In addition, the concentration of N in the inner layer part and the surface layer part can be obtained based on quantitative analysis of N using an electron beam analyzer (EPMA). In this case, the concentration distribution of N in the thickness direction of the material 1 can be obtained by performing line analysis from the surface to the inside of the material 1, and therefore the N concentrations in the inner layer portion and the surface layer portion can be efficiently obtained. .
而且,这种坯材1中,优选内层部的维氏硬度为表层部的维氏硬度的67%以上150%以下,更优选为75%以上125%以下。若内层部的N的浓度低于上述下限值、或高于上述上限值,则内层部和表层部的硬度不同,当对坯材1进行切削加工时,担心切削过程中切削性会改变。因此,有可能切出的金属框架的尺寸精度会降低。In addition, in such a material 1 , the Vickers hardness of the inner layer portion is preferably 67% to 150% of the Vickers hardness of the surface layer portion, and more preferably 75% to 125% inclusive. If the concentration of N in the inner layer is lower than the above-mentioned lower limit or higher than the above-mentioned upper limit, the hardness of the inner layer and the surface layer will be different. will change. Therefore, there is a possibility that the dimensional accuracy of the cut out metal frame will be reduced.
此外,坯材1将成为内层部和表层部的各种物理性能的差(例如,后述的切削阻力的差)小的坯材。In addition, the material 1 has a small difference in various physical properties between the inner layer portion and the surface layer portion (for example, a difference in cutting resistance to be described later).
如上所述,这种坯材1的均质性除了因为坯材1由利用粉末冶金制造的烧结体构成以外,还由来于其由从粉末制造时就在金属材料中固溶有N,并通过粉末冶金法使用该粉末制造的烧结体构成。为了粉末制造时在金属材料中固溶有N,可使用预先使原料中含有的Co、Cr、Mo和Si中至少一种氮化的方法,将原料熔融时或熔融后在氮气气氛中保持熔融金属(金属熔液)的方法,在熔融金属汇总注入氮气(鼓泡)的方法等。As mentioned above, the homogeneity of the billet 1 is not only due to the fact that the billet 1 is made of a sintered body produced by powder metallurgy, but also due to the solid solution of N in the metal material from the powder manufacturing, and through The powder metallurgy method uses the powder to produce a sintered body. In order to solid-dissolve N in the metal material during powder production, a method of nitriding at least one of Co, Cr, Mo, and Si contained in the raw material can be used in advance, and the raw material can be kept molten in a nitrogen atmosphere during or after melting. The method of metal (molten metal), the method of injecting nitrogen gas (bubbling) into the molten metal, etc.
而且,也有一种方法是通过使将金属粉末成型而得的成型体、将其烧结而成的烧结体在氮气气氛中加热、或者在氮气气氛中进行HIP处理,从而使N浸渗至合金体中(氮化处理)。然而,采用这种方法,成型体和烧结体难以从表层部至内层部均一地氮化,即便可能氮化也需要在抑制氮化速度的同时花费很长的时间,因此从坯材的制造效率的角度来看是有问题的。Furthermore, there is also a method of infiltrating N into the alloy body by heating a molded body obtained by molding metal powder or by sintering the sintered body in a nitrogen atmosphere, or by performing HIP treatment in a nitrogen atmosphere. Medium (nitrogenation treatment). However, with this method, it is difficult to uniformly nitride the molded body and the sintered body from the surface layer to the inner layer, and even if nitriding is possible, it takes a long time while suppressing the nitriding speed. It is problematic from an efficiency point of view.
另外,当对在粉末中固溶N而得的成型体进行脱脂、烧制时,通过在氮气、氩气等惰性气体中进行脱脂、烧制,从而可以抑制固溶的N的浓度变化。In addition, when degreasing and firing a molded body in which N is solid-dissolved in the powder, the change in the concentration of solid-dissolved N can be suppressed by degreasing and firing in an inert gas such as nitrogen or argon.
此外,考虑N的含有率对Si的含有率的比例(N/Si)会影响坯材1的均质性。即,当N/Si在上述范围内时,因固溶了Si而导致的晶体结构的畸变会由于固溶有N而受到抑制,其结果是,认为可提高坯材1的均质性。In addition, it is considered that the ratio of the N content to the Si content (N/Si) affects the homogeneity of the billet 1 . That is, when N/Si is within the above range, the distortion of the crystal structure due to the solid solution of Si is suppressed by the solid solution of N, and as a result, it is considered that the homogeneity of the raw material 1 can be improved.
如上所述,坯材1具有表层部与内层部之间的切削阻力的差小这一特征。因此,能够抑制对坯材1进行切削加工的过程中切削阻力发生变化,并抑制切出的金属框架的尺寸精度降低。As described above, the raw material 1 is characterized in that the difference in cutting resistance between the surface layer portion and the inner layer portion is small. Therefore, it is possible to suppress a change in cutting resistance during the cutting process of the material 1 and to suppress a reduction in the dimensional accuracy of the cut out metal frame.
具体而言,例如,当坯材1呈板状,其厚度为10mm以上时,将沿着坯材1的厚度方向的断面中,由表面至深度0.3mm的位置作为表层部,由表面至深度5mm的位置作为内层部。Specifically, for example, when the blank 1 is in the form of a plate with a thickness of 10 mm or more, the position from the surface to the depth of 0.3 mm in the section along the thickness direction of the blank 1 is taken as the surface layer part, and the position from the surface to the depth is 0.3 mm. The position of 5mm is used as the inner part.
这种情况下,优选内层部的切削阻力为表层部的切削阻力的50%以上200%以下,更优选为60%以上175%以下,进一步优选为75%以上150%以下。由此,能够抑制坯材1伴随着切削阻力的变化而出现加工精度降低。另外,若内层部的切削阻力低于上述下限值,则内层部的切削阻力与表层部的切削阻力的差会增大,因此,根据坯材1与加工工具的位置关系,担心加工精度会降低。换言之,由于内层部的切削阻力比表层部的切削阻力小很多,当例如在加工中的加工工具由表层部慢慢地向内层部移动时,切削阻力变小,有可能驱动力与切削结果之间的关联性失衡,从而出现不需要的加工。另一方面,若内层部的切削阻力高于上述上限值,则同样地,根据坯材1与加工工具之间的位置关系,加工精度有可能会降低。就是说,内层部的切削阻力比表层部的切削阻力大很多,当例如在加工中的加工工具由表层部向内层部慢慢地移动时,切削阻力增大,有可能驱动力与切削结果之间的关联性失衡,从而出现不需要的加工。In this case, the cutting resistance of the inner layer is preferably 50% to 200% of the cutting resistance of the surface layer, more preferably 60% to 175%, and still more preferably 75% to 150%. Accordingly, it is possible to suppress reduction in machining accuracy of the material 1 due to a change in cutting resistance. In addition, if the cutting resistance of the inner layer part is lower than the above-mentioned lower limit value, the difference between the cutting resistance of the inner layer part and the cutting resistance of the surface layer part will increase. Accuracy will be reduced. In other words, since the cutting resistance of the inner layer is much smaller than that of the surface layer, for example, when the processing tool in processing moves slowly from the surface layer to the inner layer, the cutting resistance becomes smaller, and it is possible that the driving force is closely related to the cutting force. The correlation between the results is out of balance, so that unwanted processing occurs. On the other hand, if the cutting resistance of the inner layer part is higher than the above-mentioned upper limit, similarly, depending on the positional relationship between the material 1 and the machining tool, machining accuracy may decrease. That is to say, the cutting resistance of the inner layer is much larger than that of the surface layer. For example, when the processing tool in processing moves slowly from the surface layer to the inner layer, the cutting resistance increases, and the driving force may be related to the cutting force. The correlation between the results is out of balance, so that unwanted processing occurs.
而且,坯材1不仅在湿式切削加工上,即便在干式切削加工上,切削阻力也比较能受到抑制,在这一点上是有用的。即,坯材1具有湿式切削加工的切削阻力与干式切削加工的切削阻力之间的差小这一特征。因此,根据由坯材1切出的金属框架的不同形状,即便是干式切削加工,也可以切出尺寸精度高的金属框架。Furthermore, the material 1 is useful in that cutting resistance can be relatively suppressed not only in wet cutting but also in dry cutting. That is, the material 1 has a feature that the difference between the cutting resistance of wet cutting and the cutting resistance of dry cutting is small. Therefore, depending on the shape of the metal frame cut out from the blank 1, even with dry cutting, it is possible to cut out a metal frame with high dimensional accuracy.
具体而言,当设湿式切削加工的切削阻力为1时,优选干式切削加工的切削阻力为2以下,更优选为1.5以下。只要干式切削加工的切削阻力相对于湿式切削加工的切削阻力在上述范围内,通过干式切削加工也可以充分地切出尺寸精度高的金属框架,因此,这种坯材1在可容易地进行切削加工这一点上是有用的。Specifically, when the cutting resistance of wet cutting is 1, the cutting resistance of dry cutting is preferably 2 or less, more preferably 1.5 or less. As long as the cutting resistance of dry cutting is within the above range relative to the cutting resistance of wet cutting, a metal frame with high dimensional accuracy can be sufficiently cut out by dry cutting. Therefore, such a blank 1 can be easily It is useful for cutting.
由于利用干式切削加工无需使用切削液,因此,具有可节约清洗切出的金属框架的工时这一优点。尤其是像金属框架这样留置于体内的情况下,由于需尽可能避免切削液的残留,因此,从切出的金属框架等的安全性的角度来看,采用干式切削加工也是有效的。Since the use of cutting fluid is not required by dry cutting, there is an advantage in that the man-hours for cleaning the cut metal frame can be saved. Especially when the metal frame is left in the body, it is necessary to avoid the residue of cutting fluid as much as possible. Therefore, dry cutting is also effective from the viewpoint of the safety of the cut metal frame.
另外,对坯材1的湿式切削加工,即使是在不用油性的切削液,而使用水溶性的切削液的情况下,也能得到良好的切削结果。由于水溶性的切削液可较容易地去除,因此,可以控制清洗的工时。而且,由于即便是在使用微量的切削液加工的半干式切削(MQL加工)时,也可得到良好的切削结果,因此,可以显著抑制切削液的使用量,同时,切出尺寸精度高的金属框架。In addition, in the wet cutting process of the material 1, good cutting results can be obtained even when a water-soluble cutting fluid is used instead of an oily cutting fluid. Since the water-soluble cutting fluid can be easily removed, the cleaning time can be controlled. Moreover, since good cutting results can be obtained even in the case of semi-dry cutting (MQL machining) that uses a small amount of cutting fluid, the amount of cutting fluid used can be significantly reduced, and at the same time, high dimensional accuracy can be cut. metal frame.
[牙科用的烤瓷用金属框架][Metal frame for dental porcelain]
下面,对本发明的牙科用的烤瓷用金属框架的实施方式进行说明。Next, an embodiment of the dental metal frame for porcelain of the present invention will be described.
图7是示出对于图1所示的坯材,本发明的牙科用的烤瓷用金属框架的实施方式在实施切出加工后的状态的立体图,图8是图7的A-A线断面图,图9是示出本发明的牙科用的烤瓷用金属框架的实施方式的纵断面图。Fig. 7 is a perspective view showing a state in which an embodiment of the metal frame for dental ceramics of the present invention is cut out of the blank shown in Fig. 1 , and Fig. 8 is a sectional view taken along line A-A of Fig. 7 , Fig. 9 is a longitudinal sectional view showing an embodiment of the metal frame for dental porcelain of the present invention.
图7所示的切削加工后的坯材1’是通过对坯材1进行切削加工而切出金属框架2的状态的坯材。金属框架2是用于作为嵌体、冠、桥、金属床、义齿、植入物、基台、夹具、螺丝等牙科用修补物的基材的构件。因此,由金属框架2可确定牙科用修补物的大概形状,因此,切出的金属框架2的形状通常为对应于所制造的牙科用修补物的形状。然后,通过在金属框架2的表面设置陶材层,可得到后述的牙科用修补物。The cut blank 1' shown in Fig. 7 is a blank in which the metal frame 2 has been cut out by cutting the blank 1. The metal frame 2 is a member used as a base material for dental prostheses such as inlays, crowns, bridges, metal beds, dentures, implants, abutments, jigs, and screws. Thus, the approximate shape of the dental prosthesis can be determined from the metal frame 2, and the shape of the cut out metal frame 2 is therefore generally corresponding to the shape of the manufactured dental prosthesis. Then, by providing a ceramic material layer on the surface of the metal frame 2, a dental prosthesis described later can be obtained.
此外,这里尤其对有关烤瓷用金属框架进行了说明,但本发明涉及的金属框架还包括不用于烤瓷的牙科用金属构件,例如嵌体、冠、桥、金属床、义齿、植入物、基台、夹具、螺丝等牙科用金属构件。In addition, metal frames for ceramics are described here, but the metal frames of the present invention also include dental metal components not used for ceramics, such as inlays, crowns, bridges, metal beds, dentures, implants , Abutments, fixtures, screws and other dental metal components.
切削加工可使用任何切削机械。例如,加工中心、铣床、钻床、车床等。其中,优选使用集成入CAM系统的切削机械。使用这样的切削机械,可使通过CAD系统等取得的模型忠实地反映在加工结果上,因此,有助于实现对患者而言安装不适感特别少的牙科用修补物。For the cutting process, any cutting machine can be used. For example, machining centers, milling machines, drilling machines, lathes, etc. Among them, it is preferable to use a cutting machine integrated into a CAM system. Using such a cutting machine can faithfully reflect a model obtained by a CAD system or the like on a machining result, and thus contributes to realization of a dental prosthesis that is particularly less uncomfortable to the patient.
图7、图8所示的切削加工后的坯材1’具有:由坯材1制得的平板部3、以及以被形成于该平板部3上的贯通孔4环绕的方式切出的金属框架2。如图8所示,在金属框架2与平板部3之间,由一小段连接部5连接,最后通过切断该连接部5,可以从切削加工后的坯材1’将金属框架2分离。The blank 1' after cutting shown in FIGS. 7 and 8 has a flat plate portion 3 made of the blank 1 and a metal cut out so as to be surrounded by a through hole 4 formed in the flat plate 3. frame 2. As shown in Fig. 8, between the metal frame 2 and the flat plate portion 3, there is a small connecting portion 5 connected, and finally by cutting the connecting portion 5, the metal frame 2 can be separated from the cut blank 1'.
图9所示的金属框架2是表示金属框架从图7、8所示的切削加工后的坯材1’分离后的状态。另外,图9所示的金属框架2的形状只是一个例子,金属框架2可根据牙科用修补物的种类形成各种形状。The metal frame 2 shown in Fig. 9 shows a state in which the metal frame is separated from the cut blank 1' shown in Figs. 7 and 8 . In addition, the shape of the metal frame 2 shown in FIG. 9 is only an example, and the metal frame 2 can be formed into various shapes according to the type of dental prosthesis.
另外,对所得的金属框架2,可以根据需要进行研磨处理。作为研磨处理,可例举例如滚磨、喷砂等处理方法。In addition, the obtained metal frame 2 may be subjected to grinding treatment as necessary. As the grinding treatment, for example, treatment methods such as barrel grinding and sand blasting may be mentioned.
而且,对所得的金属框架2还可根据需要进行二次加工。作为二次加工,可例举例如切削、磨削这样的机械加工、激光加工、电子线加工、水射流加工、放电加工、压力加工、挤压加工、轧制加工、锻造加工、弯曲加工、拉深加工、拉拔加工、滚压成型加工、剪断加工等。Moreover, secondary processing can also be performed on the obtained metal frame 2 as required. Examples of secondary processing include mechanical processing such as cutting and grinding, laser processing, electron wire processing, water jet processing, electrical discharge processing, press processing, extrusion processing, rolling processing, forging processing, bending processing, drawing, etc. Deep processing, drawing processing, roll forming processing, shearing processing, etc.
如上所述,通过这种方式得到的金属框架2具有坯材1优异的切削性,且尺寸精度高。这种金属框架2将成为可以更少的不适感安装在患部的金属框架,并能在尽量减少患者的负担的同时,如后所述,在对金属框架2的表面设置陶材层时,可得到实现陶材层的高贴紧性和高审美性的金属框架。As described above, the metal frame 2 obtained in this way has excellent machinability of the blank 1 and has high dimensional accuracy. This metal frame 2 will become a metal frame that can be installed on the affected part with less discomfort, and while reducing the burden on the patient as much as possible, as will be described later, when a ceramic material layer is provided on the surface of the metal frame 2, it can be used. A metal frame that realizes high adhesion and high aesthetics of the ceramic layer is obtained.
而且,由于金属框架2耐腐蚀性高,所以是生物体适应性优异的金属框架。Furthermore, since the metal frame 2 has high corrosion resistance, it is a metal frame excellent in biocompatibility.
而且,由于金属框架2机械特性优异,很难因咬合力而变形,因此将成为耐久性优异的金属框架。Furthermore, since the metal frame 2 has excellent mechanical properties and is hardly deformed by the occlusal force, it will be a metal frame excellent in durability.
另外,从切削加工后的坯材1’分离出金属框架2以后,剩余的平板部3除了用于其它金属框架2的切削以外,还可作为用于制造新的坯材1的原材料而回收。即,通过将剩余的平板部3熔融,并利用雾化法等进行粉末化,可得到用于坯材1的制造的金属粉末(本发明的粉末冶金用金属粉末)。In addition, after the metal frame 2 is separated from the cut blank 1', the remaining flat plate portion 3 can be used for cutting other metal frames 2, and can be recovered as a raw material for manufacturing a new blank 1. That is, the metal powder (the metal powder for powder metallurgy of the present invention) used in the production of the billet 1 can be obtained by melting the remaining flat plate portion 3 and pulverizing it by an atomization method or the like.
[牙科用修补物][Dental prosthetics]
接下来,对本发明的牙科用修补物的实施方式进行说明。Next, embodiments of the dental prosthesis of the present invention will be described.
图10是示出本发明的牙科用修补物的实施方式的纵断面图。Fig. 10 is a longitudinal sectional view showing an embodiment of the dental prosthesis of the present invention.
图10所示的牙科用修补物10包括金属框架2、以及设置用以覆盖其表面的一部分的陶材层6。A dental prosthesis 10 shown in FIG. 10 includes a metal frame 2 and a ceramic material layer 6 provided to cover a part of its surface.
陶材层6是负责牙科用修补物10的审美性的部分,一般情况下,呈现接近于牙齿颜色的颜色。The ceramic material layer 6 is a part responsible for the aesthetics of the dental prosthesis 10, and generally exhibits a color close to the color of teeth.
作为陶材层6的构成材料,可列举例如长石、石英、陶土、金属氧化物等各种陶瓷类材料、以及其他各种树脂材料等。其中,从审美性及与金属框架2的贴紧性等角度出发,优选使用陶瓷类材料。具体而言,可列举例如氧化铝、二氧化硅、氧化锂、氧化钠、氧化钾、氧化钙、氧化铁、镁、氧化锆、二氧化钛、氧化锑、氧化铈等,可使用其中的一种或二种以上的混合物。Examples of the constituent material of the ceramic layer 6 include various ceramic materials such as feldspar, quartz, clay, and metal oxides, and various other resin materials. Among them, ceramic materials are preferably used from the viewpoints of aesthetics and adhesion to the metal frame 2 . Specifically, examples thereof include alumina, silica, lithium oxide, sodium oxide, potassium oxide, calcium oxide, iron oxide, magnesium, zirconia, titanium dioxide, antimony oxide, cerium oxide, etc., and one or more of them can be used. A mixture of two or more.
将包括这种构成材料的浆料涂覆于金属框架2的表面,然后,通过进行烤瓷处理,即形成陶材层6。A paste including such a constituent material is applied to the surface of the metal frame 2, and then ceramic material layer 6 is formed by performing a ceramic treatment.
其中,陶材层6的构成材料优选包含氧化铝。当包含氧化铝的陶瓷材料被烤到金属框架2的表面上时,在陶材层6与金属框架2之间的界面附近会生成莫来石相。这种莫来石相是由于陶瓷材料方面所含的氧化铝与金属框架2方面所含的Si或氧化硅混合而生成的。因此,通过莫来石相,陶材层6与金属框架2牢牢地贴紧,陶材层6难以剥落,从而可得到可靠性高的牙科用修补物。而且,通过生成莫来石相,在烤瓷处理时,陶瓷材料对金属框架2的润湿性会提高。因此,从这一角度考虑,陶材层6的贴紧性会提高,进一步不会不均匀地烤上陶材层6。Among them, the constituent material of the ceramic material layer 6 preferably contains alumina. When a ceramic material including alumina is baked onto the surface of the metal frame 2 , a mullite phase is generated near the interface between the ceramic material layer 6 and the metal frame 2 . This mullite phase is generated by mixing alumina contained on the ceramic material side with Si or silicon oxide contained on the metal frame 2 side. Therefore, due to the mullite phase, the ceramic material layer 6 is tightly adhered to the metal frame 2, and the ceramic material layer 6 is difficult to peel off, so that a highly reliable dental prosthesis can be obtained. In addition, the generation of the mullite phase improves the wettability of the ceramic material to the metal frame 2 at the time of the porcelain firing process. Therefore, from this point of view, the adhesion of the ceramic material layer 6 is improved, and furthermore, the ceramic material layer 6 is not baked unevenly.
陶材层6的构成材料中的氧化铝的含有率优选为占质量比2%以上占质量比50%以下程度,更优选为占质量比4%以上占质量比35%以下程度,进一步优选为占质量比6%以上占质量比25%以下程度。通过将氧化铝的含有率设定在上述范围内,可确保提高陶材层6与金属框架2之间的贴紧性所需的足够的氧化铝,同时也使陶材层6自身的机械特性增强,因此,可得到可靠性更高的牙科用修补物10。The content of alumina in the constituent materials of the ceramic layer 6 is preferably at least 2% by mass and at most 50% by mass, more preferably at least 4% by mass and at most 35% by mass, and even more preferably at least 35% by mass. More than 6% by mass and less than 25% by mass. By setting the alumina content within the above-mentioned range, it is possible to ensure sufficient alumina for improving the adhesion between the ceramic material layer 6 and the metal frame 2, and at the same time, the mechanical properties of the ceramic material layer 6 itself are improved. Therefore, a more reliable dental prosthesis 10 can be obtained.
因此,若氧化铝的含有率低于上述下限值,则陶材层6与金属框架2之间不会生成足够量的莫来石相,因此,有可能陶瓷材料的润湿性会下降,陶材层6的贴紧性也会降低,另一方面,若氧化铝的含有率超过上述上限值,则机械特性容易降低,如陶材层6会变脆等,因此,还是有可能导致陶材层6的贴紧性下降。Therefore, if the content of alumina is lower than the above-mentioned lower limit, a sufficient amount of mullite phase will not be generated between the ceramic material layer 6 and the metal frame 2, so the wettability of the ceramic material may be reduced. The adhesion of the ceramic material layer 6 will also be reduced. On the other hand, if the content of alumina exceeds the above-mentioned upper limit, the mechanical properties will be easily reduced, such as the ceramic material layer 6 will become brittle. Therefore, it may still cause The adhesiveness of the ceramic material layer 6 falls.
而且,陶材层6的平均厚度不受特别限定,但优选为0.05mm以上3mm以下程度,更优选为0.2mm以上2mm以下程度。通过将陶材层6的平均厚度设定在上述范围内,能更加提高陶材层6对金属框架2的贴紧性。并且,由于陶材层6被赋予了必要且足够的遮光性,因此,金属框架2的颜色变得难以透明,从而可得到审美性优异的牙科用修补物。Furthermore, the average thickness of the ceramic material layer 6 is not particularly limited, but is preferably about 0.05 mm to 3 mm, more preferably about 0.2 mm to 2 mm. By setting the average thickness of the ceramic material layer 6 within the above range, the adhesion of the ceramic material layer 6 to the metal frame 2 can be further improved. Furthermore, since the ceramic material layer 6 is provided with necessary and sufficient light-shielding properties, the color of the metal frame 2 is less likely to be transparent, and a dental prosthesis excellent in aesthetics can be obtained.
在形成陶材层6时,首先,使用行星式磨机、球磨机等将陶材层6的构成材料磨细粉碎。然后,根据需要,在800℃以上1100℃以下、30分钟以上60分钟以下程度的范围内进行热处理。When forming the ceramic material layer 6 , first, the constituent materials of the ceramic material layer 6 are pulverized using a planetary mill, a ball mill, or the like. Then, heat treatment is performed in a range of from 800° C. to 1100° C. for 30 minutes to 60 minutes as necessary.
使由此而得的粉碎物分散于分散剂中,从而制备成糊状或浆状物。由此,可得到形成陶材层6所需的糊、浆。作为分散剂,可列举例如水、丙二醇、乙二醇、丙三醇、聚甲基丙烯酸甲酯、聚醋酸乙烯酯、硝基纤维素、乙基纤维素等。The pulverized product thus obtained is dispersed in a dispersant to prepare a paste or slurry. In this way, the paste and slurry required for forming the ceramic material layer 6 can be obtained. Examples of the dispersant include water, propylene glycol, ethylene glycol, glycerin, polymethyl methacrylate, polyvinyl acetate, nitrocellulose, ethyl cellulose and the like.
将所得的糊、浆涂覆于金属框架2的表面,进行烤瓷处理。烤瓷温度可根据陶材层6的构成材料适当设定,例如,设定为500℃以上1000℃以下。通过这种方式,可得到牙科用修补物10。The obtained paste and paste are coated on the surface of the metal frame 2, and the porcelain-fired treatment is performed. The firing temperature can be appropriately set according to the constituent materials of the ceramic material layer 6, for example, it is set at 500°C or more and 1000°C or less. In this way, a dental prosthesis 10 is obtained.
如上所述,通过优选的实施方式,已经对牙科用的被切削加工用坯材、粉末冶金用金属粉末、牙科用的烤瓷用金属框架及牙科用修补物进行了说明,但本发明不仅限于此。As mentioned above, through the preferred embodiment, the blank material to be machined for dental use, the metal powder for powder metallurgy, the metal frame for dental ceramics, and the dental prosthesis have been described, but the present invention is not limited to this.
例如,在上述实施方式中,已经对由牙科用的被切削加工用坯材切出多个牙科用的烤瓷用金属框架的情况进行了说明,但本发明不仅限于这种情况,也可适用于从一个坯材切出一个金属框架的情况。For example, in the above-mentioned embodiment, the case where a plurality of metal frames for dental ceramics are cut out from the blank to be machined for dentistry has been described, but the present invention is not limited to this case, and can also be applied In the case of cutting a metal frame from a billet.
【实施例】【Example】
接下来,对本发明的具体实施例进行说明。Next, specific examples of the present invention will be described.
1.牙科用的被切削加工用坯材的制造1. Manufacture of blanks for dental machining
(采样No.1)(Sampling No.1)
[1]首先,在高频感应炉将原材料熔化,同时通过水雾化法进行粉末化,从而得到金属粉末。接着,使用网眼150μm的标准筛分级。所得金属粉末的合金组成如表1所示。另外,N以与Cr结合的状态(氮化铬的状态)被含在原材料中。并且,合金组成的指定中,使用了SPECTRO公司制造的固体发射光谱仪(火花发射光谱仪),型号:SPECTROLAB、类型:LAVMB08A。此外,C(碳)的定量分析使用了LECO公司制造的CS-200碳硫分析装置。[1] First, the raw material is melted in a high-frequency induction furnace and powdered by the water atomization method to obtain metal powder. Next, classification was performed using a standard sieve with an opening of 150 μm. The alloy composition of the obtained metal powder is shown in Table 1. In addition, N is contained in the raw material in a state bonded to Cr (state of chromium nitride). In addition, in specifying the alloy composition, a solid-state emission spectrometer (spark emission spectrometer) manufactured by SPECTRO Corporation, model: SPECTROLAB, type: LAVMB08A was used. In addition, the quantitative analysis of C (carbon) used CS-200 carbon-sulfur analyzer manufactured by LECO company.
[2]接着,将所得的有机粘结剂溶解于水中,制备成粘结剂溶液。另外,粘结剂溶液中有机粘结剂的量为每1kg金属粉末10g。此外,粘结剂溶液中的水的量为每1g有机粘结剂50g。[2] Next, the obtained organic binder is dissolved in water to prepare a binder solution. In addition, the amount of the organic binder in the binder solution was 10 g per 1 kg of metal powder. In addition, the amount of water in the binder solution was 50 g per 1 g of the organic binder.
[3]接着,将金属粉末投入造粒装置的处理容器中。然后,在从造粒机的喷雾嘴向处理容器中的金属粉末喷洒粘结剂溶液的同时,通过喷雾干燥法将金属粉末进行造粒,从而得到造粒粉末。[3] Next, the metal powder is put into the processing container of the granulation device. Then, while spraying the binder solution onto the metal powder in the processing container from the spray nozzle of the granulator, the metal powder is granulated by a spray drying method to obtain a granulated powder.
[4]接着,使用得到的造粒粉末,在以下的成型条件下进行成型,从而得到成型体。[4] Next, using the obtained granulated powder, molding was performed under the following molding conditions to obtain a molded body.
<成型条件><Molding conditions>
·成型方法:压粉成型·Molding method: pressed powder molding
·成型压力:300MPa(3t/cm2)·Molding pressure: 300MPa (3t/cm 2 )
[5]接着,按照以下的脱脂条件,将该成型体脱脂,从而得到脱脂体。[5] Next, the molded body was degreased according to the following degreasing conditions to obtain a degreased body.
<脱脂条件><Conditions for degreasing>
·加热温度:470℃·Heating temperature: 470℃
·加热时间:1小时·Heating time: 1 hour
·加热气氛:氮气气氛· Heating atmosphere: nitrogen atmosphere
[6]接着,按照以下的烧制条件,将得到的脱脂体烧制,从而得到烧结体(牙科用的被切削加工用坯材)。所得的牙科用的被切削加工用坯材为直径100mm、厚度15mm的圆盘形。[6] Next, the obtained degreased body was fired under the following firing conditions to obtain a sintered body (material for dental machining). The obtained dental material to be machined was in the shape of a disc with a diameter of 100 mm and a thickness of 15 mm.
<烧制条件><Firing conditions>
·加热温度:1300℃·Heating temperature: 1300℃
·加热时间:3小时·Heating time: 3 hours
·加热气氛:氩气气氛Heating atmosphere: argon atmosphere
(采样No.2~No.16)(Sampling No.2~No.16)
除了使制造条件为表1所示的条件以外,其余分别与采样No.1的情况相同,从而得到了牙科用的被切削加工用坯材。Except that the manufacturing conditions were set to the conditions shown in Table 1, the rest were the same as the case of sampling No. 1, thereby obtaining dental blanks for machining.
(采样No.17~No.20)(Sampling No.17~No.20)
在高频感应炉中将原材料熔化时,在熔融金属中注入氮气。这时,通过适当改变注入时间,从而改变了N的含有率。When melting raw materials in a high-frequency induction furnace, nitrogen gas is injected into the molten metal. At this time, by appropriately changing the injection time, the N content was changed.
并且,除了其它的制造条件如表1所示以外,其余分别与采样No.1的情况相同,从而得到了牙科用的被切削加工用坯材。In addition, except that the other manufacturing conditions are as shown in Table 1, the rest were the same as the case of sample No. 1, thereby obtaining a dental blank to be machined.
(采样No.21~No.24)(Sampling No.21~No.24)
首先,使用不含N的原材料,分别与采样No.1的情况相同,从而得到了金属粉末。First, metal powders were obtained in the same manner as in the case of sample No. 1 using a raw material not containing N.
接下来,除了在使用这种金属粉末的同时,将烧制条件的加热气氛改变为占体积比50%的氩气与占体积比50%的氮气的混合气体气氛以外,其余分别与采样No.1的情况相同,从而得到了烧结体。这时,通过适当改变氮气的分压,从而改变了金属粉末中含有的N的含有率。Next, except that while using this metal powder, the heating atmosphere of the firing conditions was changed to a mixed gas atmosphere of 50% by volume of argon and 50% by volume of nitrogen, the rest were the same as the sampling No. 1, a sintered body was obtained. At this time, by appropriately changing the partial pressure of nitrogen, the content of N contained in the metal powder was changed.
并且,除了其它的制造条件如表1所示以外,其余分别与采样No.1的情况相同,从而得到了牙科用的被切削加工用坯材。In addition, except that the other manufacturing conditions are as shown in Table 1, the rest were the same as the case of sample No. 1, thereby obtaining a dental blank to be machined.
(采样No.25、No.26)(Sampling No.25, No.26)
在高频感应炉中将原材料熔化时,在熔融金属中注入氮气。这时,通过适当改变注入时间,从而改变了金属粉末中含有的N的含有率。When melting raw materials in a high-frequency induction furnace, nitrogen gas is injected into the molten metal. At this time, by appropriately changing the injection time, the content of N contained in the metal powder is changed.
并且,除了其它的制造条件如表1所示以外,其余分别与采样No.1的情况相同,从而得到了牙科用的被切削加工用坯材。In addition, except that the other manufacturing conditions are as shown in Table 1, the rest were the same as the case of sample No. 1, thereby obtaining a dental blank to be machined.
(采样No.27~No.29)(Sampling No.27~No.29)
在高频感应炉中将原材料熔化时,在熔融金属中注入氮气后,将熔融金属浇注入坯材的形状的模具中,从而得到了浇铸体。这时,通过适当改变注入时间,从而改变了金属粉末中含有的N的含有率。When melting raw materials in a high-frequency induction furnace, nitrogen gas is injected into the molten metal, and then the molten metal is poured into a mold in the shape of a billet to obtain a cast body. At this time, by appropriately changing the injection time, the content of N contained in the metal powder is changed.
并且,除了其它的制造条件如表1所示以外,其余分别与采样No.1的情况相同,从而得到了牙科用的被切削加工用坯材。In addition, except that the other manufacturing conditions are as shown in Table 1, the rest were the same as the case of sample No. 1, thereby obtaining a dental blank to be machined.
上述各采样No.的牙科用的被切削加工用坯材的制造条件如表1、2所示。Tables 1 and 2 show the manufacturing conditions of the dental workpiece blanks for each sampling No. mentioned above.
表1Table 1
表2Table 2
而且,在各表中,各个采样No.的金属粉末和牙科用的被切削加工用坯材中,对那些相当于本发明的采样,以“实施例”表示,对那些不符合本发明的采样,以“比较例”表示。In addition, in each table, among the metal powders of each sample No. and the material to be machined for dental use, those samples corresponding to the present invention are expressed as "Example", and those samples not in accordance with the present invention are expressed as "Example". , expressed as a "comparative example".
2.牙科用的被切削加工用坯材的评价2. Evaluation of raw materials for dental machining
2.1作为Si总量和氧化硅而含有的Si的含有率的测定2.1 Measurement of the Si content contained as the total amount of Si and silicon oxide
对各采样No.的牙科用的被切削加工用坯材,通过重量法及ICP发射光谱法测定了其作为Si总量和氧化硅而含有的Si的含有率。测定结果如表3所示。The content of Si contained as the total amount of Si and silicon oxide was measured by the gravimetric method and the ICP emission spectrometry for each sample No. of the dental workpiece material. The measurement results are shown in Table 3.
2.2利用X射线衍射法的结晶构造的评价2.2 Evaluation of crystal structure by X-ray diffraction method
对各采样No.的牙科用的被切削加工用坯材,进行利用X射线衍射法的结晶构造分析。然后,通过将得到的X射线衍射图谱中包含的各个峰的高度、位置与ICDD卡中登记的数据库进行对照,进行了坯材中含有的结晶构造的确定。而且,当假定起因于Co的峰中最高峰的高度为1时,算出了其起因于Co3Mo的峰中最高峰的高度的比率。计算结果如表3所示。The crystal structure analysis by the X-ray diffraction method was performed on the dental workpiece material of each sampling No. Then, the crystal structure contained in the blank was identified by comparing the height and position of each peak included in the obtained X-ray diffraction pattern with the database registered in the ICDD card. Furthermore, assuming that the height of the highest peak among the peaks derived from Co was 1, the ratio of the heights of the highest peak among the peaks derived from Co 3 Mo was calculated. The calculation results are shown in Table 3.
2.3空孔、枝晶相和结晶组织的宽高比的评价2.3 Evaluation of aspect ratio of pores, dendrite phase and crystal structure
利用切削加工,从各采样No.的牙科用的被切削加工用坯材中切出了试片。A test piece was cut out from the dental material to be machined for each sampling No. by cutting.
接着,对试片的切削面进行了研磨。然后,使用扫描电子显微镜观察研磨面,在观察图像上确定了空孔所占的区域。然后,计算测量空孔所占区域的平均直径(将其视为空孔的平均直径),同时算出了空孔所占区域的面积相对于观察图像总面积的比例(面积比)。Next, the cut surface of the test piece was ground. Then, the polished surface was observed using a scanning electron microscope, and the region occupied by the voids was identified on the observation image. Then, the average diameter of the area occupied by the measured voids was calculated (regarded as the average diameter of the voids), and the ratio of the area of the area occupied by the voids to the total area of the observed image (area ratio) was calculated.
而且,通过确认观察图像中树枝状组织究竟以多大程度存在,按照以下的评价标准,对枝晶相的存在程度进行了评价。Then, the degree of presence of the dendrite phase was evaluated in accordance with the following evaluation criteria by confirming how much the dendrite structure existed in the observation image.
<枝晶相的评价标准><Evaluation Criteria for Dendritic Phase>
◎:几乎不存在枝晶相◎: There is almost no dendrite phase
○:存在一些枝晶相(面积率为10%以下)○: Some dendrite phases exist (area ratio is 10% or less)
△:枝晶相存在稍多(面积率为10%以上20%以下)△: There are slightly more dendrite phases (the area ratio is 10% or more and 20% or less)
×:存在非常多枝晶相(面积率超过20%)×: There are very many dendrite phases (area ratio exceeds 20%)
而且,通过扫描电子显微镜观察得到的研磨面,算出观察图像上结晶组织的宽高比的平均值。Then, the obtained polished surface was observed with a scanning electron microscope, and the average value of the aspect ratio of the crystal structure on the observed image was calculated.
以上评价结果如表3所示。The above evaluation results are shown in Table 3.
2.4 N浓度的评价2.4 Evaluation of N concentration
将各采样No.的牙科用的被切削加工用坯材沿厚度方向切断,对切断面进行了研磨。The dental material to be machined for each sampling No. was cut in the thickness direction, and the cut surface was ground.
接下来,在研磨面上,利用电子束分析仪(EPMA)对坯材从表面至内部进行了线分析。并且,求得坯材的厚度方向上的N的浓度分布。Next, on the ground surface, a line analysis of the blank from the surface to the inside was carried out using an electron beam analyzer (EPMA). Furthermore, the concentration distribution of N in the thickness direction of the billet was obtained.
接下来,将由表面至0.3mm位置的N浓度作为表层部的N浓度,由表面至5mm位置的N浓度作为内层部的N浓度求出,并求出内层部的N浓度对表层部的N浓度的比例。计算结果如表3所示。Next, the N concentration from the surface to the position of 0.3 mm is taken as the N concentration of the surface layer, and the N concentration from the surface to the position of 5 mm is taken as the N concentration of the inner layer, and the N concentration of the inner layer is calculated for the N concentration of the surface layer. ratio of N concentration. The calculation results are shown in Table 3.
2.5维氏硬度的测定2.5 Determination of Vickers hardness
沿厚度方向将各采样No.的牙科用的被切削加工用坯材切断,对切断面进行研磨。Dental material to be machined for each sample No. was cut in the thickness direction, and the cut surface was ground.
接着,对研磨面中由坯材的表面至0.3mm的位置测定了维氏硬度,将其作为表层部的维氏硬度。并且,对坯材的表面至5mm的位置测定了维氏硬度,将其作为内层部的维氏硬度。Next, the Vickers hardness was measured at a position from the surface of the billet to 0.3 mm in the polished surface, and this was defined as the Vickers hardness of the surface layer. And the Vickers hardness was measured from the surface of the billet to the position of 5 mm, and this was made into the Vickers hardness of an inner layer part.
接着,求出了内层部的维氏硬度对表层部的维氏硬度的比例。计算结果如表3所示。Next, the ratio of the Vickers hardness of the inner layer portion to the Vickers hardness of the surface layer portion was obtained. The calculation results are shown in Table 3.
而且,表层部的维氏硬度的测定值如表4所示。In addition, the measured values of the Vickers hardness of the surface layer are shown in Table 4.
另外,金刚石压头的试验载荷为100gf。In addition, the test load of the diamond indenter was 100 gf.
2.6耐腐蚀性的评价2.6 Evaluation of corrosion resistance
利用切削加工,从各采样No.的牙科用的被切削加工用坯材中切出了试片。A test piece was cut out from the dental material to be machined for each sampling No. by cutting.
接着,对得到的试片,按照JIS T 6118(2012)中规定的牙科金属烤瓷修复用贵金属材料的耐腐蚀性的试验方法,测定了金属离子的溶出量。Next, the amount of eluted metal ions was measured for the obtained test pieces in accordance with the test method for corrosion resistance of precious metal materials for dental metal-ceramic restorations specified in JIS T 6118 (2012).
然后,根据如下评价标准,对测定的结果进行了评价。Then, the results of the measurement were evaluated according to the following evaluation criteria.
<耐腐蚀性的评价标准><Evaluation criteria for corrosion resistance>
◎:耐腐蚀性非常强(金属离子的溶出量非常少)◎: Very strong corrosion resistance (very little elution of metal ions)
○:耐腐蚀性强(金属离子的溶出量少)○: Strong corrosion resistance (less elution of metal ions)
△:耐腐蚀性弱(金属离子的溶出量多)△: Weak corrosion resistance (a large amount of elution of metal ions)
×:耐腐蚀性非常弱(金属离子的溶出量非常多)×: Corrosion resistance is very weak (the amount of elution of metal ions is very large)
以上的评价结果如表4所示。The above evaluation results are shown in Table 4.
2.7 0.2%耐力、伸长率和杨氏模量的测定2.7 Determination of 0.2% endurance, elongation and Young's modulus
利用切削加工,从各采样No.的牙科用的被切削加工用坯材中切出了试片。A test piece was cut out from the dental material to be machined for each sampling No. by cutting.
接着,对得到的试片,按照JIS T 6118(2012)中规定的牙科金属烤瓷修复用贵金属材料的机械性质的试验方法,测定了0.2%耐力、伸长率和杨氏模量。Next, the obtained test pieces were measured for 0.2% proof strength, elongation and Young's modulus in accordance with the test method for mechanical properties of precious metal materials for dental metal-ceramic restorations specified in JIS T 6118 (2012).
而且,按照JIS T 6004(2012)中规定的牙科金属材料的试验方法,求得了杨氏模量。Furthermore, the Young's modulus was obtained in accordance with the test method for dental metal materials specified in JIS T 6004 (2012).
测定结果如表4所示。The measurement results are shown in Table 4.
2.8疲劳强度的测定2.8 Determination of fatigue strength
利用切削加工,从各采样No.的牙科用的被切削加工用坯材中切出了试片。A test piece was cut out from the dental material to be machined for each sampling No. by cutting.
接着,对得到的试片,按照JIS T 0309(2009)中规定的试验方法,测定了疲劳强度。Next, the fatigue strength of the obtained test pieces was measured according to the test method specified in JIS T 0309 (2009).
测定结果如表4所示。The measurement results are shown in Table 4.
2.9切削性的评价2.9 Machinability evaluation
2.9.1基于切削屑的长度的评价2.9.1 Evaluation based on chip length
如下所述,对各采样No.的牙科用的被切削加工用坯材进行了切削性的评价。Machinability was evaluated for each sample No. of the dental workpiece to be machined as described below.
首先,使用钻床对得到的坯材进行孔的切削加工。接着,回收切削加工中产生的切削屑,测定其平均长度。然后,按照以下的评价标准,对测定的切削屑的平均长度进行了评价。另外,切削加工使用直径2mm的超硬合金钻头,转速为每分钟420转。此外,没有使用切削油。First, holes are cut into the obtained billet using a drill. Next, chips generated during the cutting process were recovered, and their average lengths were measured. Then, the average length of the measured chips was evaluated according to the following evaluation criteria. In addition, the cutting process uses a cemented carbide drill with a diameter of 2 mm at a speed of 420 revolutions per minute. Also, no cutting oil is used.
<切削性的评价标准><Evaluation Criteria for Machinability>
◎:切削屑的平均长度不足5mm(切削性特别好)◎: The average length of chips is less than 5mm (excellent machinability)
〇:切削屑的平均长度5mm以上且不足10mm(切削性好)〇: The average length of chips is 5 mm or more and less than 10 mm (good machinability)
△:切削屑的平均长度为10mm以上(切削性稍差)△: The average length of chips is 10 mm or more (slightly poor machinability)
×:切削屑的平均长度为10mm以上且切削屑呈螺旋状(切削性差)×: Chips with an average length of 10 mm or more and chips in a spiral shape (poor machinability)
以上评价结果如表4所示。The above evaluation results are shown in Table 4.
2.9.2基于切削阻力的评价2.9.2 Evaluation based on cutting resistance
如下所述,对通过各实施例和各比较例得到的牙科用的被切削加工用坯材进行了切削阻力的评价。The cutting resistance was evaluated for the dental blanks to be machined obtained in each of the Examples and each of the Comparative Examples as follows.
首先,将得到的坯材固定于三成分切削测力仪的测定部。First, the obtained billet was fixed to the measurement section of the three-component cutting force gauge.
接着,以沿着图6所示的轨迹扫描加工工具的方式,使用加工中心对坯材的表层部进行切削加工。然后,从切削加工中测定的三成分的切削阻力中,求得最大的值,并按照如下评价标准进行评价。Next, the surface layer portion of the blank was cut using the machining center so that the machining tool was scanned along the trajectory shown in FIG. 6 . Then, the maximum value was obtained from the cutting resistance of the three components measured during the cutting process, and evaluated according to the following evaluation criteria.
<切削阻力的评价标准><Evaluation criteria for cutting resistance>
◎:切削阻力为200N以下。◎: Cutting resistance is 200N or less.
〇:切削阻力为200N以上250N以下。〇: Cutting resistance is not less than 200N and not more than 250N.
△:切削阻力为250N以上300N以下。Δ: Cutting resistance is not less than 250N and not more than 300N.
×:切削阻力为300N以上。×: Cutting resistance is 300N or more.
以上评价结果如表4所示。The above evaluation results are shown in Table 4.
另一方面,以沿着图6所示的轨迹扫描加工工具的方式,使用加工中心对坯材的内层部进行了切削加工。然后,从切削加工中测定的三成分的切削阻力中,求得最大的值。On the other hand, the machining center was used to cut the inner layer portion of the material so that the machining tool was scanned along the trajectory shown in FIG. 6 . Then, the maximum value was obtained from the cutting resistance of the three components measured during the cutting process.
接着,算出内层部的切削阻力与先求得的表层部的切削阻力的比例。计算结果如表4所示。Next, the ratio of the cutting resistance of the inner layer part to the cutting resistance of the surface layer part obtained earlier is calculated. The calculation results are shown in Table 4.
2.10热膨胀系数的评价2.10 Evaluation of thermal expansion coefficient
利用切削加工,从各采样No.的牙科用的被切削加工用坯材中切出了试片。A test piece was cut out from the dental material to be machined for each sampling No. by cutting.
接下来,对所得的试片,按照JIS Z 2285(2003)中规定的试验方法求出热膨胀的温度依赖性。这时,通过重复温度的上升和下降,确认了热膨胀的温度依赖性的稳定性,即热膨胀系数的稳定性。然后,根据如下评价标准,对热膨胀系数的稳定性进行了评价。Next, the temperature dependence of thermal expansion was determined for the obtained test piece according to the test method specified in JIS Z 2285 (2003). At this time, by repeating the rise and fall of the temperature, the stability of the temperature dependence of thermal expansion, that is, the stability of the thermal expansion coefficient was confirmed. Then, the stability of the coefficient of thermal expansion was evaluated according to the following evaluation criteria.
<热膨胀系数的稳定性的评价标准><Evaluation Criteria for Stability of Thermal Expansion Coefficient>
◎:热膨胀系数特别稳定。◎: The coefficient of thermal expansion is particularly stable.
〇:热膨胀系数稳定。〇: The coefficient of thermal expansion is stable.
△:热膨胀系数稍微不稳定。Δ: The coefficient of thermal expansion is slightly unstable.
×:热膨胀系数不稳定。×: The coefficient of thermal expansion is unstable.
评价结果如表4所示。The evaluation results are shown in Table 4.
表3table 3
表4Table 4
由表3、表4可知,对应于各实施例的牙科用的被切削加工用坯材耐腐蚀性优异。而且,可以认为具有适当的维氏硬度,0.2%耐力、伸长率和杨氏模量均较大。As can be seen from Table 3 and Table 4, the dental blanks to be machined corresponding to the respective examples are excellent in corrosion resistance. Furthermore, it is considered that the Vickers hardness is appropriate, and the 0.2% proof strength, elongation, and Young's modulus are large.
而且,也可以认为内层部和表层部的N浓度的差、硬度的差较小。Furthermore, it is considered that the difference in N concentration and the difference in hardness between the inner layer portion and the surface layer portion are small.
而且,由于切削性优异,进行切削加工时,能够以小的切削阻力进行平滑的切削加工,且其切削阻力的变化小,因此可有效地切出所需形状。此外,由于在内层部与表层部观察到的切削阻力的差足够小,从这个角度来看,可以认为通过各实施例得到的牙科用的被切削加工用坯材能有效地切出所需形状。Moreover, due to its excellent machinability, smooth cutting can be performed with small cutting resistance during cutting, and the change in cutting resistance is small, so desired shapes can be effectively cut out. In addition, since the difference in cutting resistance observed between the inner layer part and the surface layer part is sufficiently small, from this point of view, it can be considered that the dental blanks to be machined obtained by each Example can effectively cut out the desired shape.
而且,可以认为对应于各实施例的牙科用的被切削加工用坯材包含一定量的氧化硅和空孔,同时几乎不含有枝晶相。Furthermore, it is considered that the dental workpiece materials corresponding to the respective examples contain a certain amount of silicon oxide and voids, and contain almost no dendrite phase.
另一方面,也可知对应于各比较例的牙科用的被切削加工用坯材的耐腐蚀性、机械特性和切削性均低。On the other hand, it can also be seen that the corrosion resistance, mechanical properties, and machinability of the dental blanks to be machined corresponding to the respective comparative examples are all low.
3.牙科用修补物的制造3. Manufacture of dental prostheses
利用切削加工,从各采样No.的牙科用的被切削加工用坯材中切出试片。By cutting, test pieces were cut out from the raw material to be machined for dentistry of each sampling No. .
接着,在得到的试片表面涂覆遮色瓷的糊膏,进行烧制。由此,得到了牙科用修补物的试片。Next, the paste of opaque porcelain was coated on the surface of the obtained test piece and fired. Thus, a test piece of a dental prosthesis was obtained.
另外,遮色瓷的糊膏(氧化铝含有率为占质量比15%)使用株式会社松风制造的“复古MP”。而且,烧成温度定为950℃,并在该温度下保持2分钟。此外,烧制气氛定为减压气氛。In addition, as the paste (alumina content: 15% by mass) of opaque porcelain, "Retro MP" manufactured by Matsukaze Co., Ltd. was used. Also, the firing temperature was set at 950° C., and kept at this temperature for 2 minutes. In addition, the firing atmosphere was set to be a reduced-pressure atmosphere.
4.牙科用修补物的评价4. Evaluation of Dental Prosthesis
对于在由各采样No.的坯材切出的试片上烤上遮色瓷而得到的牙科用修补物的试片,在根据JIS T 6120(2001)中规定的牙科金属烤瓷修复体的剥落和开裂发生强度试验施加破坏力的同时,也根据如下评价标准,对陶材层的贴紧性进行了评价。For the test pieces of dental prosthesis obtained by firing opaque porcelain on the test pieces cut out from the blanks of each sampling No., the peeling of dental metal-ceramic restorations specified in JIS T 6120 (2001) The adhesiveness of the ceramic layer was also evaluated according to the following evaluation criteria while applying a destructive force to the crack occurrence strength test.
<剥落/开裂发生强度试验的评价标准><Evaluation Criteria for Peeling/Cracking Incidence Strength Test>
◎:是通过采样No.27的坯材得到的试片的2倍以上。⊚: 2 times or more that of the test piece obtained by sampling the billet of No. 27.
〇:是通过采样No.27的坯材得到的试片的1.5倍以上2倍以下。〇: 1.5 times or more and 2 times or more of the test piece obtained by sampling the raw material of No. 27.
△:是通过采样No.27的坯材得到的试片的1倍以上1.5倍以下。Δ: 1 to 1.5 times that of the test piece obtained by sampling the material of No. 27.
×:是通过采样No.27的坯材得到的试片的1倍以下。x: 1 time or less of the test piece obtained by sampling the raw material of No. 27.
由表4可知,与对应于各实施例的牙科用修补物相比,对应于各实施例的牙科用修补物的陶材层的贴紧性更高。As can be seen from Table 4, compared with the dental prosthesis corresponding to each example, the adhesiveness of the ceramic material layer of the dental prosthesis corresponding to each example is higher.
而且,还将对应于各实施例的牙科用修补物切断,利用电子束分析仪对断面进行了表面分析。结果发现,在陶材层与金属框架的界面上存在层状的莫来石相。Furthermore, the dental prosthesis corresponding to each Example was cut, and the surface analysis was performed on the cross-section by an electron beam analyzer. As a result, it was found that a layered mullite phase existed at the interface between the ceramic layer and the metal frame.
并且,按照如下条件,对相当于各实施例的坯材进行了HIP处理。Furthermore, the material corresponding to each Example was subjected to HIP treatment under the following conditions.
<HIP处理条件><HIP processing conditions>
·加热温度:1100℃·Heating temperature: 1100℃
·加热时间:2小时·Heating time: 2 hours
·加压力:100MPa·Adding pressure: 100MPa
接下来,如上述2.9,对经过HIP处理的坯材进行了切削性评价。其结果是,经过HIP处理的坯材,其切削性比未经过HIP处理的坯材的切削性稍微有降低。详细原因尚未明确,但作为原因之一,可列举例如坯材的硬度会随着HIP处理而上升。Next, as in 2.9 above, machinability evaluation was performed on the HIP-treated billet. As a result, the machinability of the HIP-treated billet was slightly lower than that of the non-HIP-treated billet. The detailed reason is not clear, but as one of the reasons, for example, the hardness of the billet increases with the HIP treatment.
5.N浓度与硬度之间的关系评价5. Evaluation of the relationship between N concentration and hardness
首先,制备了具有表5所示的合金组成的各采样No.30~36的牙科用的被切削加工用坯材。First, dental workpiece blanks of Sample Nos. 30 to 36 having the alloy compositions shown in Table 5 were prepared.
接下来,按照上述“2.5维氏硬度的测定”的要点,对各采样No.30~36的牙科用的被切削加工用坯材的表层部与内层部的维氏硬度进行了测定。测定结果如表5和图11所示。Next, the Vickers hardness of the surface layer part and the inner layer part of each sample Nos. 30 to 36 of the dental workpiece to be machined was measured according to the above-mentioned "2.5 Measurement of Vickers hardness". The measurement results are shown in Table 5 and Figure 11.
表5table 5
由表5和图11可见,坯材中的N浓度和维氏硬度之间,存在有在特定的N浓度下硬度极小的关联性。如上所述,硬度减小,从而坯材的韧性增大,从而可提高拉伸强度、耐力等。并且,由N浓度测定结果可知,即使总的N浓度改变,在表层部与内层部之间也未见N浓度有显著不同。It can be seen from Table 5 and Figure 11 that there is a very small correlation between the N concentration in the billet and the Vickers hardness at a specific N concentration. As described above, the hardness decreases, so the toughness of the billet increases, so that the tensile strength, endurance, etc. can be improved. Furthermore, from the N concentration measurement results, it can be seen that even if the total N concentration is changed, there is no significant difference in N concentration between the surface layer part and the inner layer part.
符号说明Symbol Description
1、1’ 牙科用的被切削加工用坯材 2 金属框架1. 1’ Dental blank to be machined 2 Metal frame
3 平板部 4 贯通孔3 Flat part 4 Through hole
5 连接部 6 陶材层5 Connecting part 6 Ceramic layer
7 三成分切削测力仪 71 测定部7 Three-component cutting force tester 71 Measurement department
72 固定部 73 加工工具72 Fixing part 73 Processing tool
74 台 10 牙科用修补物74 sets of 10 dental restorations
11 上表面 12 下表面11 upper surface 12 lower surface
TR 轨迹。TR track.
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2015
- 2015-01-26 CN CN201510038206.8A patent/CN104818410B/en active Active
- 2015-01-30 US US14/609,861 patent/US9655698B2/en active Active
- 2015-01-30 EP EP15153311.4A patent/EP2902513A1/en not_active Withdrawn
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Also Published As
Publication number | Publication date |
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US20150216636A1 (en) | 2015-08-06 |
JP2015163732A (en) | 2015-09-10 |
US9655698B2 (en) | 2017-05-23 |
CN104818410A (en) | 2015-08-05 |
EP2902513A1 (en) | 2015-08-05 |
JP6492512B2 (en) | 2019-04-03 |
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